Patent Publication Number: US-6221938-B1

Title: Compositions of epoxysilane and reactive polymer with cure catalyst and methods of preparation

Description:
RELATED APPLICATIONS 
     This application is a divisional of U.S. application Ser. No. 08/902,127, filed Jul. 30, 1997, now U.S. Pat. No. 6,127,462, which is a continuation-in-part of application Ser. No. 08/735,055, filed Nov. 7, 1996, now U.S. Pat. No. 5,714,532, which is a continuation of application Ser. No. 08/420,389, filed Apr. 12, 1995, now abandoned. 
    
    
     BACKGROUND OF THE INVENTION 
     Conventional organic solvent based polymer compositions have become disfavored due to problems associated with environmental pollution, conservation of resources and providing a safe working environment. Instead, aqueous solution or dispersion type coating compositions have been proposed as alternatives. In particular, much attention has been paid to reactive polymer emulsions and dispersions because of the ease with which they provide improved properties such as water and solvent resistance. 
     The use of combinations of polymers, aqueous emulsions and dispersions (latices) and epoxy resins or compounds is well known in the art. For example, U.S. Pat. No. 4,049,869 to Long taught a composition including a high acid acrylic latex (5 to 20% by weight), a crosslinking agent (1 to 10%) and an ultraviolet absorber for use in preserving porous inorganic substrates. The crosslinking agent can include an epoxy resin. 
     Water-soluble silanes as additives in latex systems have also been disclosed in the prior art. For example, U.S. Pat. No. 5,017,632 to Bredow disclosed coating compositions for Portland cement or metal. The coating composition thereof can be mixed from a pair of storage stable components; a dry mix including a fine particle size filler, an epoxy resin and optionally, a coarse aggregate, and a wet mix including a polymer latex, an amine-functional epoxy curing agent, and a water-soluble epoxy- or amino-silane. 
     U.S. Pat. No. 5,100,955 to Pons disclosed coating and adhesive compositions based on aqueous dispersions of addition polymers of one or more olefinically unsaturated monomers, emulsion stabilizers and/or emulsifiers and a water-soluble epoxysilane. The water-soluble epoxysilane is added preferably after the polymerization of the addition polymer. The shelf life, however, of such compositions is only from two to three days. 
     EP Patent No. 401,496 to Hahn disclosed aqueous silicon-modified plastic dispersions as adhesives by epoxysilane-treatment of a dispersion of emulsion copolymers containing carboxylic acid, amide and sulfonic acid groups. Water soluble epoxysilanes of the formula R 1 R 2 R 3 R 4 Si are disclosed with R 1 =(cyclo)alkyl with reactive oxirane group; R 2 =(cyclo)alkoxy, (cyclo)alkyl, aryl or aralkyl; R 3 , R 4 =(cyclo)alkoxy, or OH. However, the composition of the synthetic latex is specific. Furthermore, the neat epoxysilane is added directly to the polymer. 
     In addition to these coating technologies, emulsions of trialkoxysilanes have been previously reported used as waterproofing agents. For example, buffered aqueous silane emulsions are disclosed in U.S. Pat. Nos. 4,877,654 and 5,393,330. Alkylalkoxysilanes are also emulsified with nonionic and anionic emulsifiers for water repellency properties in U.S. Pat. No. 5,226,954. 
     SUMMARY OF THE INVENTION 
     The present invention provides shelf stable compositions comprised of epoxysilane, a water dispersible or emulsifiable organic polymer which contains a functional group with an active hydrogen, together with a catalyst for curing the composition. The corresponding method of the present invention for the preparation of a shelf stable composition comprises combining an epoxysilane compound in water with the organic polymer which contains a functional group with an active hydrogen, and adding at any point a catalyst for curing the composition. 
     One embodiment of the present invention provides shelf stable compositions comprised of water-insoluble or slightly soluble epoxysilanes, emulsifier and a water dispersible or emulsifiable organic polymer which contains a functional group with an active hydrogen, together with a catalyst for curing the composition. The method of the present invention for the preparation of such a shelf stable composition comprises: (a) dispersing a water insoluble or slightly soluble epoxysilane compound in an aqueous solution with emulsifier to yield an aqueous emulsion, and (b) adding the silane emulsion to a water dispersed or emulsified organic polymer which contains a functional group with an active hydrogen, and adding at any point a catalyst for curing the composition. 
     Another aspect of the present invention is to provide an article coated and cured with any of the aforementioned reactive, aqueous compositions. 
     The compositions of the present invention are stable for at least about six (6) months. Moreover, improved properties such as solvent resistance, adhesion, smoothness, hardness and mar resistance are achieved with compositions of the present invention. 
     DETAILED DESCRIPTION OF THE INVENTION 
     The present invention provides stable epoxy silane containing compositions and methods for the preparation of stable epoxy-silane containing compositions comprising: (I) an epoxysilane, which can be a water soluble, water insoluble or slightly soluble epoxysilane; (II) optional emulsifier; (III) water; (IV) water dispersible or emulsified polymer containing a functional group with an active hydrogen; and (V) a catalyst for cure of the composition. Also provided are two part systems such that an epoxysilane emulsion comprising components (I)-(III) are combined and the components (IV) and (V) may be added upon use of components (I) to (III). Moreover, additional components, such as pH buffers may be added. Contemplated herein are also compositions for the preparation of the above compositions, namely the silane (I), the emulsifier (II), and the catalyst (V). 
     The present invention provides highly stable epoxysilane containing compositions that do not seed or gel during storage. Generally, they are stable for at least two to three weeks and more preferably two to three months. In fact, these compositions containing less than twenty weight percent epoxysilane last longer than six months of storage. This compares favorably with the prior art which taught silane/polymer compositions which would lose properties, such as adhesion, or even gel after two-three weeks. 
     The catalyst can be any that permits curing of the composition at lower temperatures, on the order of 150F., than is the case with compositions not containing the catalyst. The presence of the catalyst provides the additional advantage that one can use relatively water-soluble epoxysilanes and catalysts, thus providing greater freedom of operation and permitting the user to avoid having to use an emulsifier where such a component is not desired. 
     The cured product exhibits very satisfactory to superior properties such as high resistance to chemicals and high resistance to stains. 
     (I) SILANES 
     The epoxy functional silanes useful herein are of the general structure R 1   a R 2   b Si(OR 3 ) 4−a−b  where R 1  is an epoxy substituted alkyl or aralkyl group, where the alkyl may have from four to thirty carbon atoms, R 3  is an alkyl or alkoxy-substituted alkyl, aryl or aralkyl group having from one to ten carbon atoms, R 2  is an alkyl group or alkoxy substituted alkyl, aryl or aralkyl group having from one to ten carbon atoms, a is one to three, and b is zero to two, with the proviso that a+b is 1, 2, or 3. Each R group may be cyclic, branched or linear. Water insoluble or slightly soluble silanes useful in this invention include silanes with solubilities between 0.1 and 8.0 weight percent in water. Water insoluble epoxy silanes are preferred. However, water soluble silanes can be used although compositions made with such silanes may be less stable for extended periods of time, i.e., more than two to three days at ambient conditions. 
     The preferred epoxy functional silanes include:                    
     where: R is (CH 2 ) m , where m has a value of zero to six; 
     R 2  is an alkyl, alkoxy-substituted alkyl, aryl or aralkyl group, each of said groups having from one to ten carbon atoms; 
     R 3  is an alkyl, alkoxy-substituted alkyl, aryl or aralkyl group, each of said groups having from one to ten carbon atoms; 
     R 4 , R 5 , R 6  or R 7  are each hydrogen or an alkyl group having from one to six carbon atoms; 
     R 8  is an alkyl group having from one to four carbon atoms or aralkyl or aryl group having six to ten carbon atoms; 
     R 9  is                    
     n has a value of zero, one or two; 
     c, d and e each have a value of zero or one; and 
     f has a value of zero, one or two. 
     More specifically, R 2  denotes a substituted or unsubstituted monovalent hydrocarbon group exemplified by alkyl groups (e.g., methyl, ethyl, isobutyl, and octyl groups), alkenyl groups (e.g., vinyl and allyl groups), aryl groups (e.g., phenyl, tolyl and naphthyl groups), and aralkyl groups (e.g., benzyl and 2-phenylethyl groups), as well as those substituted groups obtained by the replacement of one or more of the carbon atoms in the above named hydrocarbon groups with various kinds of atoms and/or groups including sulfur and oxygen, and/or replacement of one or more of the hydrogen atoms in the above named hydrocarbon groups with various kinds of groups, including, but not limited to, halogen atoms, epoxy, methacryloxy, acryloxy, carboxyl, ester, cyano, and polyoxyalkylene groups. 
     R 3  are alkyl, alkoxyalkyl, aryl or aralkyl radicals such as methyl, ethyl, n-propyl, n-butyl, n-hexyl, n-heptyl, n-octyl, n-nonyl, n-decyl, and cyclo radicals such as cyclopentyl, cyclohexyl, cycloheptyl, and cyclooctyl. Illustrative of suitable branched chain hydrocarbon radicals for R 2  are alkyl radicals such as isopropyl, isobutyl, sec-butyl, isobutyl, sec-amyl, and 4-methyl-2-pentyl. Alkoxyalkyl groups may be exemplified by n-butoxy ethyl and methoxy propyl. Aryl groups may be exemplified by phenyl and aralkyl groups may be exemplified by benzyl or ethyl phenyl. 
     Water soluble epoxysilanes can be provided by formulating such that all R 3  groups are methyl. Water dispersible epoxysilanes, which are of lesser water solubility, are characterized in that the R 3  groups contain two or more carbon atoms. 
     R 4 , R 5 , R 6  or R 7  are hydrogen atoms or monovalent hydrocarbon groups having 1 to 6 carbon atoms exemplified by alkyl groups (e.g., methyl, ethyl, propyl, isopropyl, n-butyl and isobutyl groups), alkenyl groups (e.g., vinyl and allyl groups), and aryl groups (e.g., phenyl group). These hydrocarbon groups may be substituted by halogen atoms and functional groups, including cyano and epoxy, for a part or all of the hydrogen atoms therein. 
     Examples of epoxy functional silanes used in accordance with the present invention include, but are not limited to, those silanes described by Brison and Lefort in French Patent No. 1,526,231. Specific examples are 2-(3,4-epoxycyclohexyl) ethyltriethoxysilane, 4-(methyldiethoxysilyl)-1,2-epoxycyclohexane, 3-(3, 4-epoxycyclohexyl) propyl tri(isobutoxy) silane, 3-(2,3-epoxybutoxy)propyltriethoxysilane, and [2.2.1] bicycloheptane 2,3-epoxy-5-(2-triethoxysilyl)ethyl. 
     The silane(s) is present at 0.1 to 30 percent by weight of the total composition [(I)-(V)]. The preferred concentration is about 0.1 to 10 percent of the weight of the total composition. In preparing the precursor epoxy silane emulsion, as defined by components (I)-(III), the silane(s) is present at 0.1 to 60 weight percent. 
     (II) EMULSIFIER (OPTIONAL) 
     The emulsifiers for use herein, when such a component is desired, include nonionic, anionic and cationic surfactants or mixtures of nonionic with anionic or cationic surfactants. Examples of the nonionic surfactants include polyoxyethylene alkyl ethers, polyoxyethylene alkyl phenyl ethers, polyoxyethylene fatty acid esters, sorbitan fatty acid esters, and polyoxyethylene sorbitan fatty acid esters. Examples of the anionic surfactants include fatty acid salts, alkyl sulfate ester salts, alkyl benzene sulfonate, alkyl phosphate, alkylallyl sulfate ester salt, and polyoxyethylene alkylphosphate ester. Examples of the cationic surfactants include quaternary ammonium salts such as long chain alkyl trimethylammonium salts, long chain alkyl benzyl dimethyl ammonium salts, and di(long chain alkyl) dimethyl ammonium salts. A further listing of surfactants useful in the present invention may be those described in 1994 McCutcheon&#39;s Vol. 2 : Functional Materials , North American Edition (The Manufacturing Confectioner Publishing Co., Glen Rock) 1994, which is incorporated herein by reference. 
     The emulsifier(s) when used should be present in the range of 0.05 to 30 weight percent based on weight of the total composition of (I)-(V) and preferably 0.2 to 20 weight percent of the total composition. In precursor epoxysilane emulsions containing an emulsifier, the emulsifier should be present at 0.1 to 50 weight percent of the epoxy silane (I). 
     The appropriate HLB (hydrophilic-lipophilic balance) of the surfactants is chosen to correspond to the HLB of the specific epoxy silane being emulsified. The method for selecting the optimum HLB for a substance is well known to one skilled in the art and described in “The HLB System” by ICI Americas Inc. 
     Because the reactive polymer emulsion, as defined by components (II)-(IV), may be prepared prior to the addition of the precursor epoxy silane emulsion, emulsifiers of the type described above can be used in preparing these precursor compositions. Again, the emulsifiers are chosen so that the appropriate HLB is chosen to correspond to the HLB of the specific reactive polymer being emulsified with the proviso that the emulsifier(s) chosen to emulsify the reactive polymer are compatible with the emulsifier(s) used to make the precursor epoxysilane emulsion. In the precursor reactive polymer emulsion, the emulsifier should be present at 1 to 50 weight percent of the reactive polymer. 
     (III) WATER 
     The water may be present in an amount ranging from 29.85 to 99.75 weight percent of the total composition (I)-(IV). When a precursor silane emulsion is made without the polymer, about 39 to 99.75% water should be present. 
     (IV) POLYMERS 
     The reactive polymers of the present invention are those which have an active hydrogen thereon, preferably in the form of a carboxylic group. Exemplary of such polymers are those which contain terminal or pendant carboxyl groups (—COOH), some of which may be in its neutralized salt form (e.g., —COOK). These reactive polymers have molecular weights between 500 and 10 8  gms/mole. The preferred reactive polymer contains a carboxylic acid group in an amount sufficient to have an acid number, as determined by ASTM D669, between 1 and 780, and preferably, between, 10 and 280. The polymers may be added as dispersions, with no emulsifier, or as emulsions, with emulsifiers therein. 
     Examples of reactive polymers which can be used in the present invention include carboxylic acid modified polymers chosen from the following: polyethylene, polypropylene, polyethylene propylene copolymer, urethanes, epoxies, polystyrenes and urethane acrylic polymers. Also useful herein are acrylic homopolymers, vinyl acrylic polymers, methacrylic polymers, styrene acrylic copolymers, and polyesters. These reactive polymers may also contain other organic functional groups, including hydroxyl, amide, vinyl and halogens are contemplated as being within the scope of reactive polymers. 
     Specific examples of preferred reactive polymers which can be used in accordance with this invention include commercially available styrene acrylic emulsion polymers, such as JONCRYL®s 554, 540,77, and 95, and SCX 2500, all commercially available from SC Johnson Polymer of Racine, Wis. Other specific examples of commercially available preferred reactive polymers materials which can be used include NEOCRYL® acrylic emulsions, NEOREZ® water-borne urethane polymers and NEOPAC® water-borne urethane acrylic copolymers, available from ZENECA Resins of Wilmington, Mass., and UCAR® acrylic and vinyl acrylic latexes available from Union Carbide Corporation of Danbury, Conn. 
     Polymer dispersions, which contain no emulsifiers, may also be used herein. 
     The polymer should be present at 0.1 to 70 weight percent of the total composition. 
     (V) CATALYST 
     The compositions of the present invention should contain a catalyst component, composed of one or more than one catalyst capable of enabling the composition to cure faster at ambient or elevated temperatures compared to the same composition without the catalyst. 
     Several types of compounds are useful in this regard. Examples of types of useful compounds include amines, organotin compounds, organoammonium halides, and organophosphonium halides. 
     Useful amine compounds include: 
     heterocyclic amines, preferably imidazoles but also including piperazines, pyridines, and pyrrolidines, and including heterocyclic amines which are unsubstituted or substituted with one or more alkyl groups containing 1 to 6 carbon atoms, or with one or more silyl-C 1 -C 4 -alkyl groups wherein the silyl atom is substituted with a total of three substituents selected from the group consisting of alkyl and alkoxy groups containing 1 to 6 carbon atoms; preferred examples of catalysts of this type include 2-ethyl-4-methyl-1H-imidazole and 1-[3-(trimethoxysilyl)propyl}-1H-imidazole; 
     tertiary amines, wherein the nitrogen atom is substituted with a total of three substituents selected from the group consisting of alkyl containing 1 to 6 carbon atoms, unsubstituted benzyl, and benzyl substituted with one or more of alkyl containing 1 to 6 carbon atoms, hydroxyl, and dialkylaminoalkylene wherein each alkyl group contains 1 to 6 carbon atoms and the alkylene bridge contains 1 to 6 carbon atoms (preferred examples of this type of amine catalyst including N-benzyl-N-dimethylamine, and tris-2,4,6-(dimethylaminomethyl)phenol); 
     polyamides; and 
     polyalkylene polyamines, corresponding to the formula H 2 N—(ALK—NH) i —H wherein i is 1 to 10 and preferably 2-4, and each ALK is C 2 H 4 , C 3 H 6 , or C 4 H 8  and preferably C 2 H 4  (a preferred example of this type of amine catalyst being tetraethylenepentamine). 
     Useful organotin compounds include mercaptoalcohol, mercaptide or sulfide forms of diorganotin having a Sn—S or Sn═S bond. Further, illustrative examples are R 2 Sn(SCOO) type compounds, such as (n-C 4 H 9 ) 2 Sn(SCH 2 COO); R 2 Sn(SS) type compounds, such as (n-C 8 H 17 ) 2 Sn(SCH 2 COOCH 2 CH 2 OCOCH 2 S); R 2 Sn(SCH 2 COOR) 2  type compounds, such as (n-C 4 H 9 )Sn(SCH 2 COOC 8 H 17 -iso) 2 ; RSn(SCH 2 COOR) 3  type compounds, such as (n-C 4 H 9 )Sn(SCH 2 COOC 8 H 17 -iso) 3 ; R 2 Sn═S compounds, such as (n-C 8 H 17 ) 2 Sn═S or the like; and                    
     where R 5 =1-8 carbon atoms alkyl or aryl; W=—S— or —O—; and Z=—CH 2 CH(CH 2 OH)— or —CH 2 CH(OH)CH 2 —. Preferred examples are FOMREZ UL-1, UL-22, and UL-32 from Witco and dibutyltin bis(1-thioglycerol), dibutyltin oxide and dibutyltin dimercaptide. 
     Useful organoammonium halides and organophosphonium halides are Lewis acids corresponding respectively to the structures (A 1 )(A 2 )(A 3 )N-halide and (A 1 )(A 2 )(A 3 )(A 4 )P-halide wherein A 1 , A 2 , A 3  and A 4  are independently alkyl containing 1 to 4 carbon atoms, benzyl, or phenyl, and halide is chloride or bromide. The ammonium compounds are preferably substituted with at most one benzyl or phenyl group, whereas the phosphonium compounds can be substituted with 0 to 3 benzyl or phenyl groups. Preferred examples are benzyltrimethylammonium chloride and butyl-(or ethyl-)triphenylphosphonium bromide. 
     The compositions of the present invention optionally may comprise other water soluble/emulsifiable/dispersible curing catalysts, which are hydrolytically stable, to modulate the curing conditions. Examples of such catalysts are organotitanate, organotin, chelated titanium, aluminum and zirconium compounds, and combinations thereof. Examples of chelated titanates are dihydroxy bis [2-hydroxypropanato (2-)-O 1 ,O 2 ] (2-) titanate, mixed titanium ortho ester complexes, acetylacetonate chelate, bis(ethyl-3-oxobutanolato-O 1 ,O 3 ] bis(2-propanolato) titanium, isopropoxy(triethanolaminato) titanium and alkanolamine complex of titanium. Examples of organotin catalysts are FOMREZ® UL-1, UL-22, and UL-32 from Witco of Greenwich Conn. and dibutyltin bis(1-thioglycerol). 
     The catalyst can be used in an amount of 0.01 to 20 percent, preferably 0.1 to 10 parts, based on reactive polymer component (IV). 
     (VI) OPTIONAL INGREDIENTS 
     The composition of the present invention may additionally contain cross-linking agents, such as urea and melamine resins which are methylolated and/or alkoxylated, epoxy resins, aziridines and carbodiimides. Such agents may be present at 0.1 to 20 weight percent of the total composition, as long as they do not destabilize the composition during storage. 
     The pH of the total composition may impact upon its hydrostability. High alkalinity or high acidity of the composition catalyzes the hydrolysis and condensation of the alkoxysilyl group of the epoxy silane. The closer the pH of the composition is to neutral (pH=7), the better the stability of the emulsion. Therefore, the preferred range of pH of the total composition is 5.5 to 8.5. Substances which can be used to adjust the pH are organic or inorganic buffers including sodium acetate, sodium citrate, sodium carbonate, sodium bicarbonate, sodium hydrogen phosphate, sodium dihydrogen phosphate, and the corresponding potassium salts. 
     Other optional ingredients for inclusion herein are fillers, thixotropes, pigments, plasticizers, coalescing agents, biocides and fingicides as are commonly known and used in the art. 
     METHOD OF PREPARATION AND USE 
     The precursor epoxysilane compositions of the present invention are prepared by first mixing the epoxy functional silane (I) with water. If desired, an emulsifier (II) is added and the mixture is stirred to provide a white, milky emulsion. The pH of the resulting aqueous solution or emulsion is adjusted, if necessary, to pH 7.0±1.5. 
     The precursor epoxysilane solution or emulsion is added to the reactive polymer (IV) or to a reactive polymer emulsion [Components (II)-(IV)] to provide a stable composition. The method employed to mix these components is not critical and any commonly used low shear equipment, such as a blade or paddle mixer, is suitable. The catalyst (V) and any optional ingredients (VI) may be added at any time, although in some cases catalysts should be added last. 
     The solutions and emulsions may be used as two component systems, i.e., components (I)-(III) and components (IV)-(V), mixed in shortly before use, but have sufficient stability when mixed to be used as one-component systems. The composition of components (I)-(V) form uniform aqueous solutions, dispersions or emulsions. Many uses of these compositions require drying under ambient conditions or at moderately elevated temperatures (e.g., baking). The resulting dried material has excellent solvent resistance, chemical resistance, hardness, mar resistance, adhesion, water resistance, durability or weatherability. 
     The compositions made according to the present invention may be used as industrial and architectural coatings, sealants, wood coating, adhesives and in mastics, i.e., generally in any application where the polymer would be used. For example, in textile print paste applications, the composition of the present invention would provide crock resistant colorfast applications. In wood coating, the present compositions would provide stain resistance, mar resistance and block resistance between latex surfaces in storage. As to architectural coatings, the present composition would provide scrub resistance and other improved properties. In sealants, the present composition would provide adhesion to inorganic surfaces. As is clear to one of ordinary skill in the art, there is vast array of applications of the present invention in coating, sealant, adhesives, masonry sealers, fiberglass binders and sizes, inks and other water-borne polymer systems. 
    
    
     EXAMPLES 
     1. Preparation of a 40% β 3,4-epoxycyclohexyl) ethyltriethoxysilane (Silane A) Emulsion with 5% Surfactants 
     Into a beaker were added 3.85 grams of SPAN® 60 surfactant (ICI Americas) and 3.65 grams of TWEEN® 40 surfactant (ICI Americas) which were heated together in a hot water bath to melt the solid materials. 60.0 grams of Silane A were added and the mixture was stirred with a mechanical stirrer. 82.5 grams of water were added and the mixture was stirred vigorously for approximately five minutes to provide a white, stable emulsion containing 40% by weight of Silane A. 
     2. Preparation of a 20% Silane A Emulsion with 5% Surfactants 
     Into a beaker were added 3.5 grams of SPAN® 60 and 1.5 grams of TWEEN® 40 which were mixed and heated together in a hot water bath to melt the solid materials. 20.0 grams of Silane A were added and the mixture was stirred with a mechanical stirrer. 75.0 grams of water were added and the mixture was stirred vigorously for approximately five minutes to provide a white, stable emulsion containing 20% by weight of Silane A. 
     3. Preparation of a 40% Silane A Emulsion with 8% Surfactants 
     Into a beaker was added 2.18 grams of SPAN® 80 surfactant (ICI America) and 2.22 grams of TWEEN® 40 which were mixed together. To the surfactant mixture was added 22.0 grams of Silane A and the mixture was stirred with a mechanical stirrer. 28.6 grams of water were added and the mixture was stirred vigorously for approximately five minutes to provide a white, stable emulsion containing 40% by weight of Silane A. 
     4. Preparation of a 40% Silane A Emulsion with 10% Surfactants 
     Into a beaker was added 2.73 grams of SPAN® 80 and 2.77 grams of TWEEN® 40 which were mixed together. To the surfactant mixture was added 22.0 grams of Silane A and the mixture was stirred with a mechanical stirrer. 27.5 grams of water were added and the mixture was stirred vigorously for approximately five minutes to provide a white emulsion containing 40% by weight of Silane A. 
     5. Preparation of a 40% γ-glycidoxypropylmethyldiethoxysilane (Silane B) Emulsion with 8% Surfactants 
     1.93 grams of SPAN® 60 surfactant (ICI Americas) and 2.87 grams of Myrj® 52S surfactant (ICI Americas) were mixed together in a beaker and heated together in a hot water bath in order to melt the solid materials. 24.0 grams of Silane B were added and the mixture was stirred with a mechanical stirrer. 31.2 grams of water were added and the mixture was stirred for approximately thirty minutes to provide a white emulsion containing 40% by weight of Silane B. The epoxy silane emulsion was metastable and gelled within one month. 
     6. Preparation of 40% of γ-glycidoxypropyltri-(isobutoxy) Silane (Silane D) with 6 weight percent Surfactants 
     2.72 grams of SPAN® 60 surfactant and 1.18 grams of TWEEN® 40 were mixed together in a beaker and heated together in a hot water bath to melt the solid materials. 26.0 grams of D were added and the mixture was stirred with a Barhart Mixer for 20 minutes. 35.1 grams of water were added and the mixture was stirred for approximately thirty minutes to provide a white, stable emulsion containing 40% by weight of Silane D. 
     7. Preparation of 40% β-(3,4-epoxycyclohexyl)ethyl tri-(isobutoxy) Silane (Silane E) Emulsion with 6% Surfactant 
     2.36 gms of SPAN® 60 and 1.04 grams of TWEEN® 40 were mixed together in a beaker and heated together in a hot water bath to melt the solid material. 26.0 grams of Silane E were added and the mixture was stirred with a mechanical stirrer for 10 minutes. 35.1 grams of water were added and the mixture was stirred for approximately ten minutes. Giv-Gard DXN (Givaudan-Roure), a preservative, was added. 
     8-33. Preparation of Stable Epoxy Silane Containing Compositions 
     Stable epoxy silane containing compositions were prepared by adding various amounts of precursor epoxy silane emulsion (i.e., Components I-II), as prepared according to procedures described in Examples 1-7 to varying amounts of acid modified polymer dispersions (Components III-IV) or emulsions (Components II-IV). The mixtures of precursor epoxy silane emulsions and acid modified polymer dispersions or emulsions were stirred for approximately 10 minutes. The descriptions and amounts of each component of stable epoxy silane compositions are reported in Table I. 
     Comparative Examples I-XLIV 
     Comparative examples of epoxy silane acid modified polymer dispersions or emulsions were prepared by mixing various amounts of the epoxy silanes A-E and Z with varying amounts of commercially available acid modified polymer dispersions or emulsions. (see Table 1 for definition of silanes). The comparative example of alkylsilane U-W and diepoxy resin X were prepared by making an emulsion of the alkylsilanes or diepoxy resins according to procedures similar to those described in Examples 1-7, and then mixing various amounts of these alkyl silanes or diepoxy resin emulsions with varying amounts of commercially available acid modified polymer dispersions or emulsions. For example, the precursor diepoxy resin emulsion was prepared by charging into a beaker 2.44 grams of SPAN® 60 and 0.91 grams of MYR® 52S. The solids were melted by heating in a warm water bath with stirring. 18.2 grams of water were added to the mixture and stirred vigorously. 3.5 grams of 3,4 epoxycyclohexylmethyl 3,4 epoxycyclohexylcarboxylate (Union Carbide ERL-4221) were added and the mixture was stirred vigorously to yield a viscous paste. 28.7 grams of water were added and the stirring was continued for fifteen minutes to yield a white emulsion. The descriptions and amounts of each comparative example is reported in Table I. 
     
       
         
           
               
             
               
                 TABLE 1 
               
             
            
               
                   
               
               
                 Compositions of present invention (precursor epoxy emulsions 
               
               
                 and carboxylic acid modified polymers) and comparative examples. 
               
            
           
           
               
               
               
               
               
               
               
               
            
               
                 Example No. 
                 Silane 
                 % 
                 Surfactant 1   
                 % 
                 Polymer 2   
                 % 
                 Water % 
               
               
                   
               
            
           
           
               
               
               
               
               
               
               
               
            
               
                  8 
                 A 
                 0.198 
                 SPAN 60 
                 0.035 
                 JONCRYL 554 
                 46.53 
                 53.22 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.015 
                 (Acid No. 54) 
               
               
                  9 
                 A 
                 0.497 
                 SPAN 60 
                 0.087 
                 JONCRYL 554 
                 45.83 
                 53.55 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.037 
               
               
                 10 
                 A 
                 0.998 
                 SPAN 60 
                 0.175 
                 JONCRYL 554 
                 44.66 
                 54.09 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.075 
               
               
                 11 
                 A 
                 2.00 
                 SPAN 60 
                 0.192 
                 JONCRYL 554 
                 44.65 
                 52.97 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.182 
               
               
                 12 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 JONCRYL 554 
                 41.08 
                 52.94 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
               
               
                 13 
                 A 
                 0.497 
                 SPAN 60 
                 0.087 
                 JONCRYL 540 
                 42.91 
                 56.47 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.037 
                 (Acid No. 49) 
               
               
                 14 
                 A 
                 0.998 
                 SPAN 60 
                 0.175 
                 JONCRYL 540 
                 41.81 
                 56.94 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.075 
               
               
                 15 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 JONCRYL 540 
                 38.46 
                 55.56 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
               
               
                 16 
                 A 
                 2.00 
                 SPAN 60 
                 0.192 
                 JONCRYL 77 
                 45.00 
                 54.46 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.182 
                 (Acid No. 55) 
               
               
                 17 
                 B 
                 2.00 
                 SPAN 60 
                 0.161 
                 JONCRYL 77 
                 43.70 
                 53.90 
               
               
                   
                   
                   
                 MYRJ 52S 
                 0.239 
               
               
                 18 
                 A 
                 2.00 
                 SPAN 60 
                 0.197 
                 JONCRYL 95 
                 28.50 
                 69.12 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.182 
               
               
                 19 
                 B 
                 2.00 
                 SPAN 60 
                 0.161 
                 JONCRYL 95 
                 28.5  
                 69.10 
               
               
                   
                   
                   
                 MYRJ 52S 
                 0.239 
               
               
                 20 
                 A 
                 0.507 
                 SPAN 60 
                 0.089 
                 SCX 2500 
                 41.91 
                 57.09 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.038 
                 (Acid No. 19) 
               
               
                 21 
                 A 
                 1.013 
                 SPAN 60 
                 0.172 
                 SCX 2500 
                 40.82 
                 57.92 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.076 
               
               
                 22 
                 A 
                 5.045 
                 SPAN 60 
                 0.486 
                 SCX 2500 
                 37.58 
                 56.43 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.460 
               
               
                 23 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 JONCRYL 624 
                 42.83 
                 51.19 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
                 (Acid No. 50) 
               
               
                 24 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 NEOREZ R-972 
                 29.72 
                 64.30 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
                 (Acid No. 13) 
               
               
                 25 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 NEOREZ R-9679 
                 32.34 
                 61 .68 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
                 (Acid No. 23) 
               
               
                 26 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 UCAR Latex 100 
                 54.20 
                 39.83 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
                 (Acid No. 13) 
               
               
                 27 
                 A 
                 10.00 
                 SPAN 60 
                 1.203 
                 UCAR Latex 100 
                 47.24 
                 40.42 
               
               
                   
                   
                   
                 TWEEN 40 
                 1.141 
               
               
                 28 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 UCAR Latex 154 
                 52.45 
                 41.57 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
                 (Acid No.16) 
               
               
                 29 
                 A 
                 10.00 
                 SPAN 60 
                 1.203 
                 UCAR Latex 154 
                 45.71 
                 41.95 
               
               
                   
                   
                   
                 TWEEN 40 
                 1.141 
               
               
                 30 
                 A 
                 5.035 
                 SPAN 60 
                 0.485 
                 UCAR Latex 163 
                 50.70 
                 43.32 
               
               
                   
                   
                   
                 TWEEN 40 
                 0.459 
                 (Acid No.15) 
               
               
                 31 
                 A 
                 10.00 
                 SPAN 60 
                 1.203 
                 UCAR Latex 163 
                 44.19 
                 43.47 
               
               
                   
                   
                   
                 TWEEN 40 
                 1.141 
               
               
                 32 
                 B 
                 2.00 
                 SPAN 60 
                 0.160 
                 JONCRYL 77 
                 43.7  
                 53.90 
               
               
                   
                   
                   
                 MYRJ 52S 
                 0.239 
               
               
                 33 
                 B 
                 2.00 
                 SPAN 60 
                 0.160 
                 JONCRYL 95 
                 28.50 
                 69.10 
               
               
                   
                   
                   
                 MYRJ 52S 
                 0.239 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
               
               
               
               
               
             
               
                   
               
               
                 Comparative 
                   
                   
                   
                   
                   
               
               
                 Example 
                 Additive % 
                 Surfactant % 
                 Polymer 
                 % 
                 Water % 
               
               
                   
               
             
            
               
                   
               
            
           
           
               
               
               
               
               
               
               
            
               
                 I 
                 NONE 
                 NONE 
                   
                 JONCRYL 554 
                 47.00 
                 53.00 
               
               
                 II 
                 NONE 
                 NONE 
                   
                 SCX 2500 
                 43.00 
                 57.00 
               
               
                 III 
                 NONE 
                 NONE 
                   
                 JONCRYL 77 
                 46.00 
                 54.00 
               
               
                 IV 
                 NONE 
                 NONE 
                   
                 JONCRYL 540 
                 44.00 
                 56.00 
               
               
                 V 
                 NONE 
                 NONE 
                   
                 JONCRYL 95 
                 30.00 
                 70.00 
               
               
                 VI 
                 X 2.00 
                 SPAN 60 
                 0.146 
                 JONCRYL 540 
                 43.12 
                 54.63 
               
               
                   
                   
                 MYRJ 52S 
                 0.104 
               
               
                 VII 
                 X 2.00 
                 NONE 
                   
                 JONCRYL 77 
                 44.83 
                 53.17 
               
               
                 VIII 
                 A 2.00 
                 NONE 
                   
                 JONCRYL 77 
                 44.83 
                 53.17 
               
               
                 IX 
                 Y 2.00 
                 NONE 
                   
                 JONCRYL 77 
                 44.83 
                 53.17 
               
               
                 X 
                 C 2.00 
                 NONE 
                   
                 JONCRYL 77 
                 44.83 
                 53.17 
               
               
                 XI 
                 B 2.00 
                 NONE 
                   
                 JONCRYL 77 
                 44.83 
                 53.17 
               
               
                 XII 
                 Z 2.00 
                 NONE 
                   
                 JONCRYL 77 
                 44.83 
                 53.17 
               
               
                 XIII 
                 U 2.00 
                 ARQUAD 2C75 
                 0.100 
                 JONCRYL 77 
                 43.70 
                 54.10 
               
               
                   
                   
                 ARMEEN DMCD 
                 0.100 
               
               
                 XIV 
                 V 2.00 
                 SPAN 60 
                 0.206 
                 JONCRYL 77 
                 43.70 
                 53.90 
               
               
                   
                   
                 TWEEN 40 
                 0.194 
               
               
                 XV 
                 W 2.00 
                 SPAN 60 
                 0.206 
                 JONCRYL 77 
                 43.77 
                 53.90 
               
               
                   
                   
                 TWEEN 40 
                 0.194 
               
               
                 XVI 
                 Y 2.00 
                 NONE 
                   
                 JONCRYL 95 
                 29.40 
                 68.60 
               
               
                 XVII 
                 C 2.00 
                 NONE 
                   
                 JONCRYL 95 
                 29.40 
                 68.60 
               
               
                 XVIII 
                 B 2.00 
                 NONE 
                   
                 JONCRYL 95 
                 29.40 
                 68.60 
               
               
                 XIX 
                 X 2.00 
                 NONE 
                   
                 JONCRYL 95 
                 29.40 
                 68.60 
               
               
                 XX 
                 Z 2.00 
                 NONE 
                   
                 JONCRYL 95 
                 29.40 
                 68.60 
               
               
                 XXI 
                 X 2.00 
                 SPAN 60 
                 0.136 
                 JONCRYL 95 
                 28.50 
                 69.26 
               
               
                   
                   
                 MYRJ 525 
                 0.104 
               
               
                 XXII 
                 A 2.00 
                 NONE 
                   
                 JONCRYL 95 
                 29.40 
                 68.60 
               
               
                 XXIII 
                 U 2.00 
                 ARQUAD 2C75 
                 0.100 
                 JONCRYL 95 
                 28.50 
                 69.20 
               
               
                   
                   
                 ARMEEN DMCD 
                 0.100 
               
               
                 XXIV 
                 V 2.00 
                 SPAN 60 
                 0.206 
                 JONCRYL 95 
                 28.50 
                 69.10 
               
               
                   
                   
                 TWEEN 40 
                 0.194 
               
               
                 XXV 
                 W 2.00 
                 SPAN 60 
                 0.206 
                 JONCRYL 95 
                 28.50 
                 69.10 
               
               
                   
                   
                 TWEEN 40 
                 0.194 
               
               
                 XXVI 
                 A 5.00 
                 NONE 
                   
                 JONCRYL 624 
                 46.55 
                 48.45 
               
               
                 XXVII 
                 Y 5.00 
                 NONE 
                   
                 JONCRYL 624 
                 45.55 
                 48.45 
               
               
                 XXVIII 
                 A 5.00 
                 NONE 
                   
                 NEOREZ R-972 
                 32.30 
                 62.70 
               
               
                 XXIX 
                 Y 5.00 
                 NONE 
                   
                 NEOREZ R-972 
                 32.30 
                 62.70 
               
               
                 XXX 
                 A 5.00 
                 NONE 
                   
                 NEOREZ R-9679 
                 35.15 
                 59.85 
               
               
                 XXXI 
                 Y 5.00 
                 NONE 
                   
                 NEOREZ R-9679 
                 35.15 
                 59.85 
               
               
                 XXXII 
                 A 5.00 
                 NONE 
                   
                 UCAR Latex 100 
                 58.90 
                 36.10 
               
               
                 XXXIII 
                 A 10.00 
                 NONE 
                   
                 UCAR Latex 100 
                 55.80 
                 34.20 
               
               
                 XXXIV 
                 Y 5.00 
                 NONE 
                   
                 UCAR Latex 100 
                 58.90 
                 36.10 
               
               
                 XXXV 
                 Y 10.00 
                 NONE 
                   
                 UCAR Latex 100 
                 55.80 
                 34.20 
               
               
                 XXXVI 
                 A 5.00 
                 NONE 
                   
                 UCAR Latex 154 
                 57.00 
                 38.00 
               
               
                 XXXVII 
                 A 10.00 
                 NONE 
                   
                 UCAR Latex 154 
                 54.00 
                 36.00 
               
               
                 XXXVIII 
                 Y 5.00 
                 NONE 
                   
                 UCAR Latex 154 
                 51.00 
                 38.00 
               
               
                 XXXIX 
                 Y 10.00 
                 NONE 
                   
                 UCAR Latex 154 
                 54.00 
                 36.00 
               
               
                 XL 
                 A 5.00 
                 NONE 
                   
                 UCAR Latex 163 
                 55.10 
                 39.90 
               
               
                 XLI 
                 A 10.00 
                 NONE 
                   
                 UCAR Latex 163 
                 52.20 
                 37.80 
               
               
                 XLII 
                 Y 5.00 
                 NONE 
                   
                 UCAR Latex 163 
                 55.10 
                 39.90 
               
               
                 XLIII 
                 Y 10.00 
                 NONE 
                   
                 UCAR Latex 163 
                 52.20 
                 37.80 
               
               
                 XLIV 
                 X 1.00 
                 SPAN 60 
                 0.073 
                 JONCRYL 540 
                 43.05 
                 55.82 
               
               
                   
                   
                 MYRJ 52S 
                 0.051 
               
               
                   
               
               
                 A = (3,4-epoxycyclohexyl)ethyltriethoxysilane  
               
               
                 B = 3-glycidoxypropyldiethoxymethylsilane  
               
               
                 C = 3-glycidoxypropyltriethoxysilane  
               
               
                 D = 3-glycidoxypropyltri-(isobutoxy)silane  
               
               
                 E = (3,4-epoxycyclohexyl)ethyltri-(isobutoxy)silane  
               
               
                 U = octyltriethoxysilane  
               
               
                 V = 1-triethoxysilyl-2-methyldiethoxysilylethane  
               
               
                 W = amyltriethoxysilane  
               
               
                 X = (3,4-epoxycyclohexylmethyl-3,4-epoxycyclohexylcarboxylate  
               
               
                 Z = 3-glycidoxypropyltrimethoxysilane  
               
               
                   1 does not include the surfactants that may be in commercial acid modified polymer emulsion  
               
               
                   2 polymer weight is based upon solids in commercial products.  
               
            
           
         
       
     
     34-84. Shelf Life Stability 
     The shelf life stability of the stable epoxy silane emulsions containing acid modified polymer dispersions or emulsions containing acid modified polymer dispersions or emulsions (Components I-IV) and the comparative examples were determined by measuring the viscosity of these compositions at various times after preparation. The viscosity was visually monitored for flow properties by titling a bottle containing the compositions back and forth or by measuring the viscosity of the compositions at 25° C. using a Brookfield viscometer. The stabilities of the compositions are reported in Table II. 
     These examples show that the stable epoxy emulsions containing acid modified polymers (Components I-IV) are shelf stable for a period greater than 12 weeks provided that the pH of the composition is relatively neutral. For example, Example 27 has 10 weight percent Silane A and UCAR latex 100 and at a pH=6, had a viscosity of 1300 cP after storing at room temperature for 12 weeks. The compositions of comparative examples XXXIII and XXXV, where 10 percent of the Silane A was simply mixed with UCAR latex 100 showed an increase in viscosity, as shown in Examples 38 and 39, respectively. Comparative example XXXIII had an increase in viscosity to 3000 cP after storing at room temperature for 12 weeks. Comparative example XXXV gelled within 12 weeks. 
     The shelf life of the stable epoxy emulsions is important to the end use properties. For example, compositions described in Example 24 were stable for a period of 12 weeks and form a film with a smooth surface upon drying as shown in Example 67. Comparative Example XXVIII, although it did not show a change in viscosity after 12 weeks, produced a poor quality film, as shown in Example 68. This film had a cracked surface and fish eyes. The source of the surface defects was attributed to the hydrolysis and condensation of the epoxy silane to form microgels and oils. 
     The pH of the compositions can have a pronounced effect on the stability of the compositions. For example, the viscosity of compositions set forth by Example 22 gradually increased and finally gelled after 24 weeks, as shown in Example 75. The increase in viscosity was attributed to the alkalinity of the composition. The pH of the composition was 8.6. These compositions may be useful as a two-component system where long pot time is required. 
     The stability of Example 32 was observed to be poor, as shown in Example 53. Silane B is slightly soluble in water and the water solubility of this silane makes the preparation of a stable precursor epoxy emulsion difficult. The precursor epoxy silane emulsion described in Example 3 gelled within one month. Lowering the water solubility of Silane B by changing the alkoxy groups attached to the silicon atom can significantly improve the stability of the precursor epoxy silane emulsion. For example, the precursor silane emulsion described in Example 6 was stable. Of note, Silane D is insoluble in water. 
     
       
         
           
               
             
               
                 TABLE II 
               
             
            
               
                   
               
               
                 Data showing that the compositions of present invention (I-IV) form more stable mixtures than simple 
               
               
                 addition of epoxy silane or additive to aqueous emulsion or dispersion of an acid modified polymers 
               
               
                 and produce good film quality. The table also shows the effect of pH on the stability of the 
               
               
                 compositions of the present invention. 
               
            
           
           
               
               
            
               
                   
                 Viscosity of mixture (visual observation or measured 
               
               
                   
                 viscosity in cP at 25° C.) after storage at room temperature 
               
               
                   
                 for various periods of time (weeks) 
               
            
           
           
               
               
               
               
               
               
               
               
               
               
            
               
                 Example No 
                 Cmpstn 
                 pH level 
                 0 
                 1 
                 2 
                 4 
                 12 
                 24 
                 Film Quality 
               
               
                   
               
               
                 34 
                 26 
                 6.0 
                 Thin 
                   
                 Thin 
                   
                   
                   
                   
               
               
                 35 
                 XXXII 
                 6.0 
                 Thin 
                   
                 Thick 
               
               
                 36 
                 XXXIV 
                 6.0 
                 Thin 
                   
                 Thick 
               
               
                 37 
                 27 
                 6.0 
                 Thin 
                   
                   
                   
                 1300 
               
               
                 38 
                 XXXIII 
                 6.0 
                 Thin 
                   
                   
                   
                 3000 
               
               
                 39 
                 XXXV 
                 6.0 
                 Thin 
                   
                   
                   
                 gel 
               
               
                 40 
                 28 
                 4.0 
                 Thin 
                   
                 Thin 
               
               
                 41 
                 XXXVI 
                 4.0 
                 Thin 
                   
                 Thick 
               
               
                 42 
                 XXXVIII 
                 4.0 
                 Thin 
                   
                 Thick 
               
               
                 43 
                 29 
                 4.0 
                 Thin 
                   
                   
                   
                 1100 
               
               
                 44 
                 XXXVII 
                 4.0 
                 Thin 
                   
                   
                   
                 1700 
               
               
                 45 
                 XXXIX 
                 4.0 
                 Thin 
                   
                   
                   
                 2000 
               
               
                 46 
                 30 
                 4.0 
                 Thin 
                   
                 Thin 
               
               
                 47 
                 XL 
                 4.0 
                 Thin 
                   
                 Thick 
               
               
                 48 
                 XLII 
                 4.0 
                 Thin 
                   
                 Thick 
               
               
                 49 
                 31 
                 4.0 
                 Thin 
                   
                   
                   
                 1000 
               
               
                 50 
                 XLI 
                 4.0 
                 Thin 
                   
                   
                   
                 1300 
                   
               
               
                 51 
                 XLIII 
                 4.0 
                 Thin 
                   
                   
                   
                 1500 
                   
               
               
                 52 
                 16 
                 8.5 
                 Thin 
                   
                 Thin 
                   
                   
                   
                 Smooth surface 
               
               
                 53 
                 32 
                 8.5 
                 Thin 
                   
                 Gel 
                   
                   
                   
                 Smooth surface 
               
               
                 54 
                 IX 
                 8.5 
                 Thin 
                   
                 Thin 
                   
                   
                   
                 Smooth surface 
               
               
                 55 
                 X 
                 8.5 
                 Thin 
                 Gel 
                   
                   
                   
                   
                 Smooth Surface 
               
               
                 56 
                 XI 
                 8.5 
                 Thin 
                   
                 Gel 
                   
                   
                   
                 Smooth Surface 
               
               
                 57 
                 VI 
                 8.5 
                 Thin 
                   
                   
                 Gel 
                   
                   
                 Smooth Surface 
               
               
                 58 
                 18 
                 8.5 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Smooth Surface 
               
               
                 59 
                 33 
                 8.5 
                 Thin 
                   
                   
                 Separate into 
                   
                   
                 Smooth Surface 
               
               
                   
                   
                   
                   
                   
                   
                 2 layers 
                   
                   
               
               
                 60 
                 XVI 
                 8.5 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Cratered Surface 
               
               
                 61 
                 XVII 
                 8.5 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Smooth Surface 
               
               
                 62 
                 XVIII 
                 8.5 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Cratered Surface 
               
               
                 63 
                 XXI 
                 8.5 
                 Thin 
                   
                   
                 Separated into 
                   
                   
                 Smooth surface 
               
               
                   
                   
                   
                   
                   
                   
                 2 layers 
                   
                   
               
               
                 64 
                 23 
                 8.0 
                 Thin 
                   
                   
                 Thick 
                   
                   
                 Smooth surface 
               
               
                 65 
                 XXVI 
                 8.0 
                 Thin 
                   
                 Gel 
                   
                   
                   
                 Gel particles &amp; 
               
               
                   
                   
                   
                   
                   
                   
                   
                   
                   
                 cratered 
               
               
                 66 
                 XXVII 
                 8.0 
                 Thin 
                   
                   
                 Thick 
                   
                   
                 Rough cratered 
               
               
                   
                   
                   
                   
                   
                   
                   
                   
                   
                 surface 
               
               
                 67 
                 24 
                 8.0 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Smooth Surface 
               
               
                 68 
                 XXVIII 
                 8.0 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Fish eyes, cracked 
               
               
                   
                   
                   
                   
                   
                   
                   
                   
                   
                 surface 
               
               
                 69 
                 XXIX 
                 8.0 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Cratered surface 
               
               
                 70 
                 25 
                 8.0 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Smooth surface 
               
               
                 71 
                 XXX 
                 8.0 
                 Thin 
                   
                   
                 Thin 
                   
                   
                 Fish eyes 
               
               
                 72 
                 XXXI 
                 8.0 
                 Thin 
                   
                   
                 Thick 
                   
                   
                 Fish eyes 
               
               
                 73 
                 20 
                 8.5 
                  50 
                  49 
                  50 
                   
                   
                  63 
               
               
                 74 
                 21 
                 8.5 
                  65 
                  62 
                  64 
                   
                   
                  75 
               
               
                 75 
                 22 
                 8.6 
                 148 
                 146 
                 107 
                   
                   
                 gel 
               
               
                 76 
                 II 
                 8.5 
                  28 
                  30 
                  29 
                   
                   
                  45 
               
               
                 77 
                 13 
                 8.6 
                  28 
                  30 
                  29 
                   
                   
                 400 
               
               
                 78 
                 14 
                 8.6 
                 135 
                 154 
                 192 
                   
                   
                 440 
               
               
                 79 
                 15 
                 8.6 
                 149 
                 260 
                 913 
                   
                   
                 gel 
               
               
                 80 
                 IV 
                 8.6 
                 228 
                 206 
                 208 
                   
                   
                 240 
               
               
                 81 
                 9 
                 8.4 
                 924 
                 396 
                 493 
                   
                   
                 260 
               
               
                 82 
                 10 
                 8.5 
                 234 
                 378 
                 500 
                   
                   
                 930 
               
               
                 83 
                 12 
                 8.5 
                 193 
                 860 
                 5675  
                   
                   
                 gel 
               
               
                 84 
                 I 
                 8.5 
                    4.13 
                 397 
                 423 
                   
                   
                 520 
               
               
                   
               
            
           
         
       
     
     85-111. Solvent Resistance 
     The stable epoxy silane emulsions containing acid modified polymers are useful in improving the solvent resistance of films cast from them. The solvent resistance was determined by methyl ethyl ketone (MEK) double rubs. The tests were conducted according to ASTM D4752-87. Films were cured at 23° C. and 50% relative humidity for seven days or cured at 121° C. for 20 minutes and then 23° C. at 50% relative humidity for 7 days. The results of solvent resistance is reported in Table III. 
     The solvent resistance of films cast from compositions of the present invention was significantly better than films cast from the acid modified polymers alone. For example, the number of MEK double rubs of a film cast from compositions described in Example 16 and shown in Example 90 and cured at 121° C. for 20 minutes was 130 rubs. Comparative Example III, a film of JONCRYL 77 withstood only 11 MEK rubs, as shown in Example 91. Simple mixtures of Silane A and JONCRYL 77, Comparative Example VIII, withstood only 34 rubs. In some cases, simple blends of epoxy silanes and polymers, such as Comparative Example XI, yield solvent resistant films shown in Example 94, but the shelf life of these compositions is poor. For example, Comparative Example XI gelled in two weeks, as shown in Example 56/ 
     
       
         
           
               
             
               
                 TABLE III 
               
             
            
               
                   
               
               
                 Data showing that the compositions of present invention have improved solvent resistance, as 
               
               
                 demonstrated by MEK double rubs 
               
            
           
           
               
               
            
               
                   
                 MEK double rubs 
               
            
           
           
               
               
               
               
            
               
                   
                   
                 Cured at 23° C. at 50% 
                 Cured at 121° C. for 20 min. and then 
               
               
                 Example No. 
                 Composition 
                 relative humidity for 7 days 
                 23° C. at 50% relative humidity for 7 days 
               
               
                   
               
               
                 85 
                  8 
                 29 
                 39 
               
               
                 86 
                  9 
                 — 
                 40 
               
               
                 87 
                 10 
                 26 
                 — 
               
               
                 88 
                 11 
                 — 
                 50 
               
               
                 89 
                 I 
                 14 
                  9 
               
               
                 90 
                 16 
                 41 
                 130  
               
               
                 91 
                 III 
                 14 
                 11 
               
               
                 92 
                 IX 
                 41 
                 169  
               
               
                 93 
                 XII 
                 110  
                 171  
               
               
                 94 
                 XI 
                 87 
                 127  
               
               
                 95 
                 VI 
                  8 
                  9 
               
               
                 96 
                 VII 
                   
                 45 
               
               
                 97 
                 VIII 
                   
                 34 
               
               
                 98 
                 XIII 
                 — 
                 11 
               
               
                 99 
                 XIV 
                 — 
                  9 
               
               
                 100  
                 XV 
                 — 
                  9 
               
               
                 101  
                 18 
                 19 
                 182  
               
               
                 102  
                 V 
                  8 
                  7 
               
               
                 103  
                 XVI 
                  2 
                 22 
               
               
                 104  
                 XX 
                 57 
                 241  
               
               
                 105  
                 XVIII 
                 — 
                 22 
               
               
                 106  
                 XXI 
                 12 
                 22 
               
               
                 107  
                 XIX 
                 — 
                 46 
               
               
                 108  
                 XXII 
                 — 
                 51 
               
               
                 109  
                 XXIII 
                 — 
                 14 
               
               
                 110  
                 XXIV 
                 — 
                 13 
               
               
                 111  
                 XXV 
                 — 
                  8 
               
               
                   
               
               
                 1. Film had craters.  
               
            
           
         
       
     
     112-115. Mar Resistance. 
     The compositions of the present invention have improved mar resistance when cast as films. The mar resistance was measured using an AATCC crockmeter, Atlas Electric Devices Company, model CM-5. Films were cast into Bonderite treated cold-rolled steel panels using a draw down bar and cured at 121° C. for 20 minutes and 23° C. and 50% relative humidity for seven days. The gloss values were determined according to ASTM D 523. The results of the mar resistance of these films are reported in Table IV. Films cast from compositions of the present invention demonstrated an improvement in mar resistance for compositions freshly prepared and aged 6 months (Examples 112 and 113) as compared to compositions from Comparative Examples XLIV and IV (Examples 114 and 115). 
     
       
         
           
               
             
               
                 TABLE IV 
               
             
            
               
                   
               
               
                 Data showing that the mar resistance of 
               
               
                 films cast from compositions of present 
               
               
                 inventions are better than simple mixture 
               
               
                 of epoxy silane and acid modified polymers 
               
            
           
           
               
               
               
               
               
            
               
                 Example 
                   
                 Initial 
                 Gloss after 
                   
               
               
                 No. 
                 Composition 
                 Gloss (60°) 
                 10 cycles 
                 % loss 
               
               
                   
               
               
                 112 
                 14 1   
                  96 
                 32 
                 67 
               
               
                 113 
                 14 2   
                 100 
                 50 
                 50 
               
               
                 114 
                 XLIV 
                  98 
                 26 
                 73 
               
               
                 115 
                 IV 
                 103 
                 24 
                 77 
               
               
                   
               
               
                   1 film cast immediately after preparation of composition  
               
               
                   2 film cast 6 months after preparation of composition.  
               
            
           
         
       
     
     116-125. Hardness 
     Films cast from the compositions of the present invention had an increase in hardness while maintaining other film properties, such as gloss, and adhesion, as indicated in Table V. Pencil hardness was measured according to ASTM D 3363-74. The gloss was measured according to ASTM-D 523. Crosscut tape adhesion was measured according to ASTM 3359-90. Wet adhesion of the film to E-coat steel panel was measured according to Method 6301 of US Federal Standard Test Method 141B. The films were prepared using a draw down bow. The dry film thickness was 2 mils. The films were cured at 121° C. for 20 minutes and 23° C. and 50% relative humidity for 7 days. 
     
       
         
           
               
             
               
                 TABLE V 
               
             
            
               
                   
               
               
                 Data showing that composition of present invention give a 
               
               
                 good balance of film properties after curing at 
               
               
                 121° C. for 2 minutes and 23° for 7 days 
               
            
           
           
               
               
               
               
               
               
            
               
                   
                 Compo- 
                 Gloss value 
                 Hardness 
                 Tape 
                 Wet 
               
            
           
           
               
               
               
               
               
               
               
            
               
                 Example 
                 sition 
                 20° 
                 60° 
                 Pencil 
                 Adhesion 
                 Adhesion 
               
               
                   
               
               
                 116 
                 16 
                 84 
                 97 
                 HB 
                 5B 
                 10 
               
               
                 117 
                 17 
                 78 
                 99 
                 H 
                 5B 
                 10 
               
               
                 118 
                 XII 
                 64 
                 92 
                 F 
                 5B 
                 10 
               
               
                 119 
                 VI 
                 80 
                 99 
                 B 
                 5B 
                 10 
               
               
                 120 
                 III 
                 89 
                 105  
                 B 
                 5B 
                 10 
               
               
                 121 
                 18 
                 80 
                 94 
                 2H 
                 5B 
                 10 
               
               
                 122 
                 19 
                 64 
                 92 
                 F 
                 5B 
                 10 
               
               
                 123 
                 XX 
                 80 
                 99 
                 HB 
                 5B 
                 10 
               
               
                 124 
                 XXI 
                 80 
                 99 
                 HB 
                 5B 
                 10 
               
               
                 125 
                 V 
                 96 
                 107  
                 B 
                 5B 
                 10 
               
               
                   
               
            
           
         
       
     
     A dramatic illustration of the usefulness of the composition of the present invention is presented for a filled latex sealant. The sealant formulations are set forth in Table VI. The sealants were prepared by charging UCAR latex polymer 105 and TRITON X-405 into a mixing vessel and stirring for five minutes. A solution of NUOCEPT 95 preservative, TRITON X-405 surfactant and water was added to the mixing vessel and stirred for five minutes. The ethylene glycol, TEMOL 850 dispersing agent, ASE 60 thickener, KTPP potassium tripolyphosphate, and SANTICISER 160 plasticizer were added and mixed using a high speed mixing propeller. Mineral spirits, precursor epoxy silane emulsion or silicone additive and ammonium hydroxide were added and mixed using a spatula. A MOLTINI PLANAMAX mixer was used to stir the mixture for 20 minutes under a nitrogen atmosphere. The TiO 2  and DMDEE (2,2-dimorpholino diethyl ether) catalysts were added and mixed for five minutes. The mixture was degassed under reduced pressure for five minutes. The sealant was stored in a plastic sealant tube. 
     The sealants were cured at 23° C. and 50% relative humidity for three weeks in an environmental chamber and 1 week at ambient conditions. The physical properties of the cured sealants were measured according to ASTM D 412C (percent elongation, tensile strength and modulus), ASTM 624 (tear strength), C-661 (shore A hardness) and C-794 (adhesion in peel). 
     The sealants were heat aged at 50° C. for 4 weeks. The physical properties of the sealant are reported in Table VI. The compositions of the present invention, when fully formulated into a filled acrylic latex (Example 129), had excellent adhesion while maintaining high elongation and low modulus, especially after aging for 4 weeks at 50° C. The comparative examples 126-28, 130-31 had either poor adhesion after heat aging or dramatic loss of percent elongation. 
     
       
         
           
               
             
               
                 TABLE VI 
               
             
            
               
                   
               
               
                 Data showing that the compositions of the present invention 
               
               
                 give a good balance of properties in a filled latex selant 
               
               
                 LATEX SEALANT FORMULATIONS 
               
            
           
           
               
               
               
            
               
                 Components 
                 Parts 
                 Source 
               
               
                   
               
               
                 1. FILLED FORMULATION 
                   
                   
               
               
                 UCAR ® Latex Polymer 105 
                 200.00  
                 Union Carbide 
               
               
                 TRITON ® X-405 
                 3.45 
                 Union Carbide 
               
               
                 (70% Active Surfactant) 
               
               
                 NUOSEPT ® 95 (Preservative) 
                 0.50 
                 Huls 
               
               
                 TRITON ® X 405 
                 0.50 
                 Union Carbide 
               
               
                 Distilled Water 
                 0.50 
               
               
                 Ethylene Glycol 
                 4.95 
                 Aldrich 
               
               
                 TEMOL ® 850 (Dispersing Agent) 
                 0.50 
                 Rohm &amp; Haas 
               
               
                 ASE ® 60 (Thickener) 
                 4.00 
                 Rohm &amp; Haas 
               
               
                 KTPP (Potassium Tripolyphosphate) 
                 0.50 
                 FMC 
               
               
                 SANTICISER ® 160 (Plasticizer) 
                 50.00 
                 Monsanto 
               
               
                 Mineral Spirits 
                 4.00 
                 Aldrich 
               
               
                 Organofunctional Silane or precursor 
                 2.00 
                 OSi Specialties 
               
               
                 epoxy emulsion 
               
               
                 Ammonium Hydroxide (28% Soln) 
                 1.00 
                 Fisher 
               
               
                 DRIKALITE ® 
                 230.00  
                 ECC 
               
               
                 (Treated Calcium Carbonate) 
               
               
                 Titanium Dioxide R-901 
                 4.00 
                 DuPont 
               
               
                 DMDEE (Catalyst) 
                 0.50 
                 Texaco 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
            
               
                   
               
               
                 PHYSICAL PROPERTIES a  FOR FILLED ACRYLIC 
               
               
                 LATEX SEALANT FORMULATION 
               
            
           
           
               
               
               
               
               
               
               
               
               
            
               
                   
                   
                   
                   
                   
                   
                   
                 Adhesion 
                   
               
               
                   
                   
                   
                   
                   
                   
                   
                 to 
               
               
                   
                   
                   
                   
                   
                   
                   
                 Anodized 
                 Cohesive 
               
               
                   
                   
                 Elongation 
                 Tensile 
                 Modulus 
                 Tear 
                 Hardness 
                 Aluminum 
                 Failure 
               
               
                 Example 
                 Silane 
                 % 
                 (psi) 
                 (Young&#39;s) 
                 (lbs/in) 
                 (Shore A) 
                 (lbs/in) 
                 Mode (%) 
               
               
                   
               
               
                 126 
                 None 
                   
                   
                   
                   
                   
                   
                   
               
               
                   
                 Initial 
                 400 
                 44.8 
                 43.3 
                 19.7 
                  6 
                 8.1 
                 65% 
               
               
                   
                 Aged b   
                 347 
                 41.2 
                 29.0 
                 20.1 
                 15 
                 9.5 
                 10    
               
               
                 127 
                 Z 
               
               
                   
                 Initial 
                 287 
                 62.4 
                 39.3 
                 22.9 
                 20 
                 7.2 
                 95% 
               
               
                   
                 Aged 
                 158 
                 110.6  
                 119.4  
                 30.1 
                 15 
                 5.8 
                 98% 
               
               
                 128 
                 A 
               
               
                   
                 Initial 
                 300 
                 72.6 
                 36.2 
                 26.6 
                 23 
                 4.4 
                 100%  
               
               
                   
                 Aged 
                  70 
                 116.3  
                 313.8  
                 16.4 
                 16 
                 3.4 
                 100%  
               
               
                 129 
                 Example 1 
               
               
                   
                 Initial 
                 300 
                 73.3 
                 41   
                 36.5 
                 15 
                 7.7 
                 93% 
               
               
                   
                 Aged 
                 199 
                 82.5 
                 60.6 
                 29.1 
                 22 
                 11.2  
                 90% 
               
               
                 130 
                 W 
               
               
                   
                 Initial 
                 567 
                 27.4 
                  9.3 
                  9.3 
                 15 
                 5.1 
                 20% 
               
               
                   
                 Aged 
                 200 
                 125.3  
                 25.5 
                 25.5 
                 24 
                 7.5 
                  7% 
               
               
                 131 
                 T 
               
               
                   
                 Initial 
                 253 
                 53.2 
                 26.9 
                 26.9 
                 28 
                 9.1 
                 100%  
               
               
                   
                 Aged 
                 219 
                 39.1 
                 20.2 
                 20.2 
                 21 
                 8.0 
                 20% 
               
               
                   
               
               
                   a Physical properties measurements obtained in accordance with accepted ASTM test specifications;  
               
               
                   b Samples were aged for four (4) weeks at 50° C.;  
               
               
                 A = (3,4-epoxycyclohexyl)ethyltriethoxysilane  
               
               
                 T = 3-aminopropylsiloxanes in water  
               
               
                 Z = 3-glycidoxypropyltrimethoxysilane  
               
               
                 Example 1. Precursor epoxy silane emulsion prepared in Example 1  
               
               
                 W = amyltriethoxysilane. (The silane was added as an emulsion prepared by mixing 40 grams of amyltriethoxysilane, 4.11 grams of SPAN 60 and 3.87 grams of TWEEN 40 and 52 grams of water.)  
               
            
           
         
       
     
     EXAMPLES USING AMINE CATALYSTS 
     The following examples demonstrate the very satisfactory and superior results obtained when an amine catalyst is present in the composition, in accordance with the present invention. 
     The tests were carried out using either a commercially available styrene acrylic latex sealer/topcoat with an acid number of 10.7, termed “Latex X” hereinafter, or “Rhoplex CL-204” (Rohm &amp; Haas), both of which are commercial acrylic latexes with pendant carboxylic groups. 
     In each test, the components indicated were combined, the resulting composition was cured, and the properties of the cured product were determined 4 hours, 3 days, and 7 days later. The test procedures were as described hereinabove. 
     Amine catalysts identified by product name are: 
     
       
         
           
               
               
             
               
                   
               
             
            
               
                 Anquamide 360 (Air Products) 
                 Polyethylene polyamine, polyamide 
               
               
                   
                 solution 
               
               
                 Anquamine 401 (Air Products) 
                 Tetraethylene pentamine 
               
               
                 EMI-24 (Air Products) 
                 2-Ethyl-4-methyl-1H-imidazole 
               
               
                 DMP-30 and DY-064 (Ciba, now 
                 Tris-2,4,6-(dimethylaminomethyl)- 
               
               
                 Novartis) 
                 phenol 
               
               
                 BMDA and DY-062 (Ciba, now 
                 N-Benzyl-N-dimethylamine 
               
               
                 Novartis) 
               
               
                 PE-1013 (ELF Atochem) 
                 Dibutyltin bis(1-thioglycerol) 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% [14.89% Anquamide 360/water] + 
               
               
                 3% of 40% emulsion of Silane “Y − 1” 
               
               
                 (α-[3,4-epoxycyclohexyl]-ethyl triethoxysilane) 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 14.89% Anquamide 360/water. 
                 9.33 
               
               
                 Latex X + 1% of [14.89% Anquamide 360/Water]. 
                 7.9  
               
               
                 Latex X + 1% of [4.89% 
               
               
                 Anquamide 360/water + 3% of 40% Y − 1 emulsion. 
                 7.81 
               
               
                 1% of 14.89% Anquamide 360/water was added with 
               
               
                 1.74% Dowanol PnB to Latex X [No gel particles were present] 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS 15 min. 
               
               
                 baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance 
               
               
                 Test 
               
               
                 at 50° C. for 2 hr. 
                 2 lb 
                 2 
                  8 
                  9 
               
               
                   
                 4 lb 
                 2 
                  8 
                  7 
               
               
                 At Room 
                 2 lb 
                 10 
                 10 
                 10 
               
               
                 Temp. [4 hr.] 
                 4 lb 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 HB 
                 B 
               
               
                 Methyl Ethyl ketone 
               
               
                 Resistance Test [Double 
                   
                 31 
                 76 
                 181  
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.3 
                   1.8 
                   1.9 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% [28.89% Anquamine 401/water] + 
               
               
                 3% of 40% Y − 1 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 Latex X + 1% Anquamine 401 
                 8.47 
               
               
                 Latex X + 1% Anquamine 401 + 
               
               
                 3% of 40% Y − 1 emulsion 
                 8.55 
               
               
                 CURING CYCLE FOR COATED PANELS: 
                 15 min. baked @ 150° F., 
               
               
                 Cured for: 
               
               
                   
               
            
           
           
               
            
               
                 CURING TIME AT 
               
               
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance 
               
               
                 Test 
               
               
                 At 50° C. for 
                 2 lb. 
                  5 
                  9 
                  9 
               
               
                 2 hr 
                 4 lb. 
                  2 
                  9 
                  7 
               
               
                 At Room 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                 Temp. [4 hr.] 
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 HB 
                 HB 
                 HB 
               
               
                 Methyl Ethyl 
                   
                 21 
                 61 
                 &gt;400  
               
               
                 Ketone 
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.5 
                   1.8 
                   1.9 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% EMI-24 + 3% of 40% Y-1 emulsion. 
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 SAMPLES 
                 pH 
               
               
                   
                   
               
               
                   
                 Latex X 
                 6.78 
               
               
                   
                 Lalex X + 1% EMI-24 
                 8.97 
               
               
                   
                 Latex X + 1% EMI-24 + 3% of 40% Y-1 emulsion 
                 8.91 
               
               
                   
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 6 
                 9 
                 9 
               
               
                   
                 4 lb. 
                 3 
                 8 
                 9 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 F 
                 F 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 72 
                 241 
                 &gt;400 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.3 
                 1.8 
                 1.9 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% Ethyltriphenylphosphinium 
               
               
                 Bromide + 3% of 40% Y-1 emulsion. 
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 SAMPLES 
                 pH 
               
               
                   
                   
               
               
                   
                 Latex X 
                 6.78 
               
               
                   
                 Latex X + 1% Ethyltriphenylphosphonium Bromide 
                 6.48 
               
               
                   
                 Latex X + 1% Ethyltriphenylphosphonium Bromide + 
                 6.51 
               
               
                   
                 3% of 40% Y-1 emulsion. 
               
               
                   
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 7 
                 7 
                 7 
               
               
                   
                 4 lb. 
                 7 
                 7 
                 7 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 B 
                 2B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 38 
                 56 
                 171 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.7 
                 1.5 
                 1.8 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% DMP-30 + % of 40% Y-1 emulsion. 
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 SAMPLES 
                 pH 
               
               
                   
                   
               
               
                   
                 Latex X 
                 6.78 
               
               
                   
                 Latex X + 1% DMP-30 
                 9.65 
               
               
                   
                 Latex X + 1% DMP-30 + 3% of 40% Y-1 emulsion. 
                 9.6 
               
               
                   
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 7 
                 5 
                 5 
               
               
                   
                 4 lb. 
                 3 
                 3 
                 3 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 2B 
                 3B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 32 
                 78 
                 128 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.9 
                 1.05 
                 1.8 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% BMDA + 3% of 40% Y-1 emulsion. 
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 SAMPLES 
                 pH 
               
               
                   
                   
               
               
                   
                 Latex X 
                 6.78 
               
               
                   
                 Latex X + 1% BMDA 
                 8.69 
               
               
                   
                 Latex X + 1% BMDA + 3% of 40% Y-1 emulsion. 
                 8.69 
               
               
                   
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 6 
                 7 
                 5 
               
               
                   
                 4 lb. 
                 3 
                 7 
                 7 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 B 
                 B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 26 
                 78 
                 102 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.6 
                 1.9 
                 1.9 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% (Butyl)triphenylphosphonium 
               
               
                 Bromide + 3% of 40% Y-1 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 Latex X + 1% (Butyl)triphenylphosphonium Bromide 
                 6.38 
               
               
                 Latex X + 1% (Butyl)triphenylphosphonium Bromide + 3% of 
                 6.44 
               
               
                 40% Y-1 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 4 
                 7 
                 8 
               
               
                   
                 4 lb. 
                 3 
                 7 
                 8 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 2B 
                 B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 38 
                 140 
                 157 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.8 
                 1.9 
                 1.8 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% Benyltrimethylammonium Chloride + 
               
               
                 3% of 40% Y-1 emulsion. 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 Latex X + 1% Benzyltrimethylammonium Chloride 
                 6.49 
               
               
                 Latex X + 1% Benzyltrimrthylammonium Chloride + 3% of 40% 
                 6.52 
               
               
                 Y-1 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 4 
                 7 
                 7 
               
               
                   
                 4 lb. 
                 1 
                 5 
                 7 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 8 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 &gt;5B 
                 4B 
                 2B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 25 
                 28 
                 29 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.8 
                 2 
                 1.7 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 0.2% Tin [II] Chloride + 3% of 40% 
               
               
                 Y-1 emulsion. 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.68 
               
               
                 Latex X + 0.2% Tin [II] Chloride 
                 3.89 
               
               
                 Latex X + 0.2% Tin [II] Chloride + 3% of 40% Y-1 emulsion 
                 3.95 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 7 
                 6 
                 6 
               
               
                   
                 4 lb. 
                 3 
                 3 
                 5 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 B 
                 HB 
                 HB 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 38 
                 35 
                 43 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.8 
                 1.3 
                 1.1 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% of 50% Accelerator DY 062/water + 
               
               
                 3% of 40% Y-1 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 50% Accelerator DY-062/water [Insoluble] 
                 10.9 
               
               
                 50% Accelerator DY-062/water + 20% Acetic acid [Soluble]. 
                 7.45 
               
               
                 Latex X + 1% of 50% Accelerator DY 062/water/Acetic acid 
                 6.43 
               
               
                 Latex X + 1% of 50% Accelerator DY 062/water/Acetic acid + 3% 
                 6.5 
               
               
                 of 40% Y-1 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 4 
                 5 
                 6 
               
               
                   
                 4 lb. 
                 4 
                 1 
                 5 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 2B 
                 B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 49 
                 52 
                 72 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.8 
                 1.3 
                 1.6 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% of 25% Fomrez UL-22 emulsion + 3% 
               
               
                 of 40% Y-1 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 25% Fomrez UL-22 emulsion [25% Fomrez UL-22 + 35.5% 
                 6.23 
               
               
                 Igepal CA-897 (Non Ionic surfactant) + 39.5% water. 
               
               
                 Latex X + 1% of 25% Fomrez UL-22 emulsion. 
                 6.84 
               
               
                 Latex X + 1% of 25% Fomrez UL-22 emulsion + 3% of 40% 
                 6.75 
               
               
                 Y-1 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 4 
                 7 
                 8 
               
               
                   
                 4 lb. 
                 2 
                 3 
                 6 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 2B 
                 B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 59 
                 114 
                 130 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.9 
                 1.7 
                 1.7 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% of 25% PE-1013 [Tin catalyst] 
               
               
                 emulsion + 3% of 40% Y-1 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 25% PE-1013 emulsion [25% PE-1013 (Tin catalyst) + 35.5% 
                 6.61 
               
               
                 Igepal CA-897 (non Ionic surfactant) + 39.5% water. 
               
               
                 Latex X + 1% of 25% PE-1013 emulsion. 
                 6.86 
               
               
                 Latex X + 1% of 25% PE-1013 emulsion + 3% of 40% Y-1 
                 6.86 
               
               
                 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 2 
                 5 
                 5 
               
               
                   
                 4 lb. 
                 2 
                 2 
                 4 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 2B 
                 B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 65 
                 69 
                 278 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.8 
                 1.5 
                 2.1 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 0.5% Dowanol PnB.[Control] 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X + 0.5% Dowanol PnB. 
                 6.78 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 min. baked @ 150° F., 
               
               
                 Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance 
               
               
                 Test 
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                  9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 HB 
                 B 
                 HB 
               
               
                 Methyl Ethyl Ketone 
                   
                 28 
                 27 
                 28 
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.1 
                   1.3 
                   1.7 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 3% of 40% Y − 1 emulsion 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.78 
               
               
                 Latex X + 3% of 40% Y − 1 emulsion. 
                 6.94 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE : 15 min. baked @ 150° F., 
               
               
                 Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance 
               
               
                 Test 
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                  5 
                  5 
                 10 
               
               
                   
                 4 lb. 
                  1 
                  1 
                  9 
               
               
                 At Room 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                 Temp. [4 hr.] 
                 4 lb. 
                  9 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 2B 
                 F 
               
               
                 Methyl Ethyl Ketone 
                   
                 32 
                 40 
                 46 
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.7 
                   1.4 
                   1.2 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description : Latex X + 1% DY 064 [catalyst] + 
               
               
                 3% of 40% Y − 1 emulsion 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.68 
               
               
                 Latex X + 1% DY 064 [catalyst]. 
                 9.48 
               
               
                 Late`x + 1% DY 064 + 3% of 40% Y − 1 emulsion. 
                 9.39 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE : 15 min. baked @ 150° F., Cured 
               
               
                 for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance Test 
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 6 
                  5 
                  3 
               
               
                   
                 4 lb. 
                 1 
                  1 
                  2 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 2B 
                 HB 
               
               
                 Methyl Ethyl Ketone 
                   
                 51  
                 53 
                 78 
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                    1.63 
                   1.7 
                   1.9 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% of 20% DY 95771 
               
               
                 Dowanol PnB + 3% of 40% Y − 1 emulsion 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.68 
               
               
                 Latex X + 1% of 20% DY 95771 Dowanol PnB. 
                 6.59 
               
               
                 Latex X + 1% of 20% DY 95771 Dowanol PnB + 
                 6.66 
               
               
                 3% of 40% Y − 1 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE : 15 min. baked @ 150° F., 
               
               
                 Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance 
               
               
                 Test 
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                  5 
                  5 
                  3 
               
               
                   
                 4 lb. 
                  1 
                  1 
                  1 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 2B 
                 HB 
               
               
                 Methyl Ethyl ketone 
                   
                 28 
                 28 
                 27 
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.4 
                   1.8 
                   1.3 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% of 65% Dibutyl 
               
               
                 Tin Oxicle Dispersion + 3% of 40% Y − 1 emulsion 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.68 
               
               
                 65% Dibutyl Tin Oxide Dispersion [lot #52- 
                 9.22 
               
               
                 4] 
               
               
                 Latex X + 1% of 65% Dibutyl Tin Oxide Dispersion 
                 6.89 
               
               
                 Latex X + 1% of 65% Dibutyl Tin Oxide Dispersion + 
                 7.16 
               
               
                 3% of 40% Y − 1 emuision 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE : 15 min. baked @ 150° F., Cured 
               
               
                 for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance Test 
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                  5 
                  8 
                  9 
               
               
                   
                 4 lb. 
                  3 
                  6 
                  8 
               
               
                 At Room Temp.[4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 HB 
                 HB 
               
               
                 Methyl Ethyl ketone 
                   
                 66 
                 160  
                 160  
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.5 
                   1.5 
                   1.8 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL - 204, Formulation 
               
               
                 WR - 204 - 2 [no additive] 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex CL 204 
                 6.72 
               
               
                 Rhoplex WR - 204 - 2 
                 8.1  
               
               
                 [Formulated] 
               
               
                   
               
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance Test 
               
               
                 at 5° C. for 2 hr. 
                 2 lb 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb 
                 10 
                 10 
                 10 
               
               
                 AT Room Temp.[4 hr.] 
                 2 lb 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 B 
                 2B 
               
               
                 Methyl Ethyl Ketone 
                   
                 19 
                 17 
                 19 
               
               
                 Resistance Test 
               
               
                 [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   2.8 
                   1.7 
                   2.8 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL - 204, Formulation WR - 204 - 2 + 
               
               
                 3% of 40% emulsion of silane “Y − 2” 
               
               
                 [2-(3,4-Epoxycyclohexyl)ethyltriethoxysilane] 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex CL 204 
                 6.72 
               
               
                 Rhoplex WR - 204 - 2 [Formulated] 
                 8.1  
               
               
                 Rhoplex WR- 204 - 2 + 3% Y − 
                 8.13 
               
               
                 2 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 15 min. baked @ 150° F., 
               
               
                 Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance 
               
               
                 Test 
               
               
                 At 5° C. for 2 hr. 
                 2 lb. 
                 10 
                  9 
                 10 
               
               
                   
                 4 lb. 
                  9 
                  9 
                 10 
               
               
                 At Room 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                 Temp. [4 hr.] 
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 B 
                 B 
                 B 
               
               
                 Methyl Ethyl 
                   
                 33 
                 30 
                 149  
               
               
                 Ketone 
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.5 
                   1.9 
                   1.4 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL 204, Formulation 204 - 2 +1% 
               
               
                 Benyltrimethylammonium Chloride + 3% of 40% Y − 2 emulsion 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex CL 204 
                 6.72 
               
               
                 Rhoplex WR 204 - 2 
                 8.1  
               
               
                 Rhoplex WR 204 - 2 + 1% Benzyltrimethylammonium Chloride 
                 8.2  
               
               
                 Rhoplex WR 204-2 + 1% Benzyltrimethylammonium Chloride + 
                 8.35 
               
               
                 3% of 40% Y − 2 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 15 min. 
               
               
                 baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance Test 
               
               
                 At 5° C. for [2 hr.] 
                 2 lb. 
                  8 
                  8 
                  9 
               
               
                   
                 4 lb. 
                  7 
                  7 
                  8 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                  8 
                  0 
                 10 
               
               
                 Pencil Hardness 
                   
                 &gt;5B 
                 3B 
                 2B 
               
               
                 Methyl Ethyl ketone 
                   
                 23 
                 29 
                 32 
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.5 
                   1.7 
                   1.9 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL -204, Formulation 204 -2 + 0.4% 
               
               
                 (Ethyl)triphenylphosphonium Bromide + 3% of 40% Y − 2 emulsion 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR 204 - 2 
                 8.1 
               
               
                 Rhoplex WR - 204 - 2 + 0.4% (Ethyl) triphenylphosphonium 
               
               
                 Bromide 
               
               
                 [5% (Ethyl)triphenylphosphonium Bromide + 81.94% water + 1.85% 
                 8.4 
               
               
                 Arcosolve DPTB, +3.71% Arcosolve DPM and 7.5% Butyl 
               
               
                 Propasol.]Rhoplex WR - 204 - 2 + .4% 
               
               
                 (Ethyl) triphenylphosphonium Bromide 
               
               
                 [58% (Ethyl) triphenylphosphonium Bromide + 81.94% water + 
                 8.5 
               
               
                 1.85% Arcosolve DPTB, 3.71% Arcosolve DPM and 7.5% 
               
               
                 Butyl Propasol]+ 3% of 40% Y − 2 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 15 min. 
               
               
                 baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance Test 
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                  9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                  8 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 B 
                 B 
                 B 
               
               
                 Methyl Ethyl Ketone 
                   
                 24 
                 70 
                 207  
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.8 
                   1.5 
                   1.6 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL 204, Formulation WR 204 -2 + 
               
               
                 1% EMI - 24 [15% EMI - 24/Water] + 3% of 40% Y − 2 emulsion 
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR 204 - 2 
                 8.1  
               
               
                 Rhoplex WR 204 - 2 + 1% EMI - 24 
                 8.75 
               
               
                 [15% EMI - 24] 
               
               
                 Rhoplex WR - 204 - 2 + 1% 
               
               
                 EMI - 24 + 3% of 40% Y − 2 
                 8.86 
               
               
                 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE, FOR COATED PANELS: 15 min. baked @ 
               
               
                 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
               
            
               
                   
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
               
               
                 Print Resistance Test 
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                  9 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 B 
                 B 
                 B 
               
               
                 Methyl Ethyl Ketone 
                   
                 21 
                 219  
                 &gt;400  
               
               
                 Resistance Test [Double 
               
               
                 Rubs] 
               
               
                 Coating Thickness [mils.] 
                   
                   1.5 
                   1.6 
                   1.6 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex WR-204-2 + 1% N-Benzyl-N- 
               
               
                 Dimethylamine (BMDA) [50% BMDA, 3.7% Arcosolve DPTB, 7.4% 
               
               
                 Arcosolve DPM and 38.9% Butyl Propasol] + 3% of 40% Y-2 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR-204-2 
                 8.1 
               
               
                 Rhoplex WR-204-2 + 1% N-Benzyl-N-Dimethylamine [BMDA] 
                 8.9 
               
               
                 [50% BMDA, 3.7% Arcosolve DPTB, 7.4% Arcosolve DPM, and 
               
               
                 38.9% Butyl Propasol] 
               
               
                 Rhoplex WR-204-2 + 1% N-Benzyl-N-Dimethylamine [BMDA] 
                 8.9 
               
               
                 [50% BMDA, 3.7% Arcosolve DPTB, 7.4% Arcosolve DPM, and 
               
               
                 38.9% Butyl Propasol] + 3% of 40% Y-2 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 B 
                 HB 
                 HB 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 26 
                 68 
                 192 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.9 
                 1.9 
                 1.7 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL-204 (Unformulated Resin) + 0.4% 
               
               
                 (Butyl)triphenylphosphonium Bromide [2.66% Butyltriphenyl- 
               
               
                 phosphonium Bromide, 24.75% Arcosolve DPM, 12.34% Arcosolve 
               
               
                 DPTB, 50.05% Butyl Propasol and 10.2% Water] + 3% of 40% 
               
               
                 Y-2 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex CL-204 (unformulated) 
                 6.78 
               
               
                 Rhoplex CL-204 (Unformulated, pH adjusted to 8.5 with 14% 
                 8.5 
               
               
                 Ammonium Hydroxide solution.) 
               
               
                 Rhoplex CL-204 [pH 8.5, Unformulated] + 0.4% (Butyl)- 
                 7.9 
               
               
                 triphenylphosphinium Bromide [2.66% (Butyl)triphenyl- 
               
               
                 phosphonium Bromide] 
               
               
                 Rhoplex CL-204 [pH 8.5, Unformulated] + 0.4% (Butyl)- 
                 8.01 
               
               
                 triphenylphosphinium Bromide [2.66% (Butyl)triphenyl- 
               
               
                 phosphonium Bromide] + 3% of 40% Y-2 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 2 
                 9 
                 6 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 B 
                 HB 
                 B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 48 
                 48 
                 231 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.7 
                 1.9 
                 1.3 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex WR-204-2 + 1% of 9.49% Anquamide 
               
               
                 360 [Anquamide 9.49%, Arcosolve DPTB, 18% Butyl Propasol 68.91%, 
               
               
                 Water 4.59%] + 3% of 40% Y-2 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR-204-2 
                 8.1 
               
               
                 Rhoplex WR-204-2 + 1% of Anquamide 360 [Anquamide 
                 8.2 
               
               
                 9.49%, Arcosolve DPTB 18%, Butyl Propasol 68.91%, Water 
               
               
                 4.59%] 
               
               
                 Rhoplex WR-204-2 + 1% of Anquamide 360 + 3% of 40% Y-2 
                 8.26 
               
               
                 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 5 
                 9 
                 9 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 F 
                 F 
                 F 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 18 
                 31 
                 139 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.6 
                 1.7 
                 1.6 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL-204-2 + 1% of a 20% formulation of 
               
               
                 silane “Y-3” {1-[3-(trimethoxysilyl)propyl]-1H-imidazole} (The emulsion 
               
               
                 consisted of {20% silane Y-3, Ethanol 200 proof 53.3%, Distilled water 
               
               
                 17.78%, Glacial Acetic acid 8.89%. The pH of the mixture was adjusted to 
               
               
                 8.5-9.0 with conc. Ammonium Hydroxide] + 3% of a 40% emulsion of 
               
               
                 silane Y-2. 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex CL-204-2 
                 8.1 
               
               
                 Rhoplex CL-204-2 + 1% of a 20% formulation of silane Y-2 
                 8.3 
               
               
                 Rhoplex CL-204-2 + 1% of a 20% formulation of silane Y-3 + 
                 8.3 
               
               
                 3% of a 40% emulsion of silane Y-2 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 B 
                 F 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 72 
                 219 
                 &gt;400 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.5 
                 1.6 
                 1.9 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex WR-204-2 + 1% of the 20% formulation of 
               
               
                 Y-3 + 3% of the 40% emulsion of silane Y-2 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR-204-2 
                 8.1 
               
               
                 Rhoplex WR-204-2 + 1% of 20% formulation of Y-3 
                 8.3 
               
               
                 Rhoplex WR-204-2 + 1% of 20% formulation of Y-3 + 
                 8.3 
               
               
                 of 40% emulsion of Y-2 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 [Non Baked] @ Ambient Temp., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 B 
                 B 
                 F 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 28 
                 52 
                 &gt;400 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.5 
                 1.3 
                 1.4 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex WR-204-2 + 1% Anquamine-401 
               
               
                 [15% Anquamine] and 85% water] + 3% of 40% Y-2 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR-204-2 
                 8.2 
               
               
                 Rhoplex WR-204-2 + 1% Anquamine-401 [15% Anquamine-40 
                 8.6 
               
               
                 and 85% water] 
               
               
                 Rhoplex WR-204-2 + 1% Anquamine-401 [15% Anquamine and 
                 8.76 
               
               
                 85% water] + 3% of 40% Y-2 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE FOR COATED PANELS: 
               
               
                 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME AT 
               
               
                   
                 AMBIENT TEMP. 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 6 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 F 
                 F 
                 F 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 27 
                 28 
                 142 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.8 
                 1.7 
                 1.8 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex WR-204-2 + 1% EMI [50% EMI + 
               
               
                 25% Ethanol + 25% water] and 3% of 40% Y-1 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR-204-2 
                 8.1 
               
               
                 Rhoplex WR-204-2 + 1% EMI [50% EMI + 25% Ethanol + 
                 8.2 
               
               
                 25% water] 
               
               
                 Rhoplex WR-204-2 + 1% EMI [50% EMI + 25% Ethanol + 
                 8.2 
               
               
                 25% water] and 3% Y-1 emulsion] 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 min. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 9 
                 9 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 2B 
                 2B 
                 HB 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 62 
                 73 
                 &gt;400 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.7 
                 1.2 
                 1.6 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex WR-204-2 + 1% EMI [50% EMI + 
               
               
                 25% Ethanol + 25% water] and 3% of 40% Y-1 emulsion} 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Rhoplex WR-204-2 
                 8.1 
               
               
                 Rhoplex WR-204-2 + 1% EMI [50% EMI + 25% Ethanol + 
                 8.2 
               
               
                 25% water] 
               
               
                 Rhoplex WR-204-2 + 1% EMI [50% EMI + 25% Ethanol + 
                 8.2 
               
               
                 25% water] and 3% Y-1 emulsion 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: Non baked @ Room Temperature, Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 9 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 8 
                 9 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 3B 
                 B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 37 
                 45 
                 &gt;400 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.3 
                 1.7 
                 1.3 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Rhoplex CL-204-2 + 1% silane Y-3 
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 SAMPLES 
                 pH 
               
               
                   
                   
               
               
                   
                 Rhoplex WR-204-2 
                 8.1 
               
               
                   
                 Rhoplex CL-204-2 + 1% Silane Y-1 
                 8.3 
               
               
                   
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 mins. baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 6 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 3 
                 10 
                 10 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 2B 
                 2B 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 20 
                 20 
                 19 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.5 
                 1.2 
                 1.5 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% of the 20% formulation of Y-3 + 
               
               
                 3% of the 40% emulsion of Y-2 
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 SAMPLES 
                 pH 
               
               
                   
                   
               
               
                   
                 Latex X 
                 6.61 
               
               
                   
                 Latex X + 1% of 20% Y-3 formulation 
                 6.13 
               
               
                   
                 Latex X + 1% of 20% Y-3 formulation + 3% of 40% Y-2 
                 6.13 
               
               
                   
                 emulsion. 
               
               
                   
                   
               
            
           
           
               
            
               
                 CURING CYCLE: 15 mins baked @ 150° F., Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 7 
                 7 
                 7 
               
               
                   
                 4 lb. 
                 5 
                 5 
                 9 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 HB 
                 HB 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 32 
                 55 
                 &gt;400 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.6 
                 1.2 
                 1.5 
               
               
                   
               
            
           
         
       
     
     
       
         
           
               
             
               
                   
               
             
            
               
                 Sample Description: Latex X + 1% of the 20% formulation of Y-3 + 
               
               
                 3% of the 40% Y-2 emulsion 
               
               
                   
               
            
           
           
               
               
            
               
                 SAMPLES 
                 pH 
               
               
                   
               
               
                 Latex X 
                 6.61 
               
               
                 Latex X + 1% of 20% Y-3 formulation 
                 6.13 
               
               
                 Latex X + 1% of 20% Y-3 formulation + 3% of 40% Y-2 emulsion 
                 6.13 
               
               
                   
               
            
           
           
               
            
               
                 CURING CYCLE: Non baked @ Room Temperature, Cured for: 
               
            
           
           
               
               
            
               
                   
                 CURING TIME 
               
            
           
           
               
               
               
               
            
               
                   
                 .17 day 
                 3 days 
                 7 days 
               
               
                   
                   
               
            
           
           
               
               
               
               
               
            
               
                 Print Resistance Test 
                   
                   
                   
                   
               
               
                 At 50° C. for [2 hr.] 
                 2 lb. 
                 7 
                 8 
                 7 
               
               
                   
                 4 lb. 
                 5 
                 7 
                 7 
               
               
                 At Room Temp. [4 hr.] 
                 2 lb. 
                 10 
                 10 
                 10 
               
               
                   
                 4 lb. 
                 10 
                 10 
                 10 
               
               
                 Pencil Hardness 
                   
                 3B 
                 HB 
                 HB 
               
            
           
           
               
               
               
               
            
               
                 Methyl Ethyl Ketone Resistance 
                 30 
                 51 
                 &gt;400 
               
               
                 Test [Double Rubs] 
               
               
                 Coating Thickness [mils.] 
                 1.4 
                 1.6 
                 1.7