Use of additives to breakdown and stabilize wax during fiber recycle

Methods for controlling wax and other contaminants by improving the dispersion of these materials through the addition of treatment agents such as plasticizers, dispersants or wetting agents to the process of recycling paper and paperboard are disclosed. Preferred treatment agents include polymeric wetting agents, dispersants, plasticizers and combinations thereof.

FIELD OF THE INVENTION 
Methods for controlling wax and other contaminants by improving the 
dispersion of these materials through the addition of treatment agents 
such as plasticizers, dispersants or wetting agents to the process of 
recycling paper and paperboard are disclosed. Preferred treatment agents 
include polymeric wetting agents, dispersants, plasticizers and 
combinations thereof. 
BACKGROUND OF THE INVENTION 
Old corrugated containers (OCC) make up a high percentage of the recycled 
paper used in the United States, a majority of which is made into new 
container board. With such a high reuse level, old corrugated containers 
are an extremely important raw material for the container board industry. 
A significant unused source of OCC are wax treated containers. These are 
corrugated containers which are coated or impregnated with wax and used to 
ship fruit, produce and other agricultural products, as well as 
nonagricultural products such as bulk nail, screw, and bearing boxes. With 
waxed corrugated representing about 1.3 million tons or about 5% of the 
shipped corrugated in 1995, it represents an attractive fiber source. What 
makes this source even more attractive is the fact that waxed corrugated 
is typically produced from virgin fiber and its use is concentrated in a 
handful of industries; thus it is a high quality fiber source that would 
be relatively inexpensive to collect. Currently, waxed corrugated is not 
accepted for recycling. It is considered too contaminated and is sorted 
out for landfilling or sold for its b.t.u. value. The problem is that 
waxed corrugated causes a serious contamination issue for a mill. The 
released wax tends to collect on equipment and in the finished paper 
products causing problems with mill operations and affecting product 
quality. To reasonably increase the level of waxed OCC used by the paper 
industry to the point where mills will accept and possibly seek out waxed 
containers, great strides in new technology for controlling wax in the 
recycle plant will have to be introduced. 
Wax is a generic term widely applied to a diverse group of natural and 
synthetic products which have similar physical characteristics; they are 
plastic solids at ambient temperatures, and low viscosity fluids at 
moderately elevated temperatures. The chemical composition of waxes can be 
complex, containing a variety of molecular weight species and functional 
groups, or relatively simple, as in the case of some petroleum and 
synthetic waxes which are composed solely of hydrocarbons. Natural waxes 
are derived from various sources such as insects, animals, vegetables, 
minerals, and petroleum. Examples of synthetic waxes include low molecular 
weight polyethylene (mol. wt.&lt;600), solid polyethylene glycols, amide 
waxes, and Fisher-Tropsch waxes (low molecular weight polymethylene). 
Depending on the specific application, waxed corrugated containers will be 
coated with blends of paraffin and micro waxes as well as blends that 
include synthetic waxes, polymers, and resins. Synthetic waxes such as 
polyethylene and Fischer-Tropsch are similar to paraffin wax in that they 
are composed of unbranched alkanes, but because they're polymeric 
materials they tend to have much higher molecular weights. For example, 
polyethylene waxes are composed of low molecular weight polyethylenes, and 
Fisher-Tropsch are low molecular weight polymethylenes. Melting points for 
these materials tend to be significantly greater than those for petroleum 
waxes (&gt;200.degree. F. for polyethylene and up to 220.degree. F. for 
Fisher-Tropsch polymers), thus their addition to a wax will produce higher 
melting points and often increased coating hardness. The most common 
polymer additive to be incorporated into wax coatings is ethylene-vinyl 
acetate (EVA). EVA is a random copolymer of ethylene (50-95%) and 
vinylacetate (5-50%). EVAs with softening points of up to 400.degree. F. 
are often used. 
Wax-blend coatings may also include tackifying resins which are 
incorporated to increase the affinity of the wax coating for a substrate. 
In addition to the adhesional effects, the added resins can also lower a 
coating's softening and melting points. Tackifying resins include 
hydrocarbons, rosins and rosin derivatives, and polyterpenes. Hydrocarbon 
resins can be aliphatic or aromatic hydrocarbons. Aliphatic rosins include 
low molecular weight polymers and alkenes with 5-carbon backbones. 
Aromatic hydrocarbon resins are 9-carbon derivatives of polystyrene. 
Rosins are free acids and acids containing double bonds. They're naturally 
occurring resins which are found in pine trees. Derivatives are produced 
by polymerizing, hydrogenating, or estifying rosin. Polyterpenes are 
derived from alpha- or beta-pinene. 
In the recycle plant, mill operators have defined three categories for the 
wax that is removed from the OCC at the repulper: free wax which is 
removed from boxes as large discrete particles, suspended wax which exist 
as small dispersed particles (in the 40 micrometer range), and adsorbed 
wax which coats the fibers. The distribution amongst these categories will 
depend on the repulping temperatures, the melting point of the coatings, 
and the temperature of the pulp slurry as it moves through the recycle 
plant. A typical recycle mill will repulp OCC at temperatures of around 
115-140.degree. F. For some coated containers, this may be hot enough to 
melt or suspend the wax and completely defiber the waxed corrugated 
containers. The low viscosity of the suspended wax allows for the 
formation of small, discrete particles which move freely with the pulp 
slurry. These particles are removed at high efficiencies during the 
washing or dewatering of the pulp, but as the temperature drops, they can 
again solidify and adhere to fibers (adsorbed wax) and mill equipment. At 
the typical wax-based (contamination) level in OCC, this only periodically 
affects operations. However, when levels of treated containers increase 
(e.g., when grocery store bails which typically contain a high wax-coated 
container concentration enter the system), the higher levels of wax 
results in more frequent shutdowns (breaks and clean-ups) and lower 
quality product. 
In addition to appearance problems from wax spotting in final products, the 
wax associated with the fiber can interfere with the performance of 
additives such as sizing agents and retention aids. It can also affect the 
handling, conversion, and performance of the final product. The wax lowers 
the paper-to-paper friction coefficient. In the industry, this is 
typically quantified as the tangent of the angle at which two paper 
surfaces will begin to slide free from each other, known as the angle of 
slip (AOS), or slide angle. There is strong evidence that wax is the 
primary cause of reduced AOS in board utilizing OCC. This reduced friction 
coefficient can create problems during conversion. For example, the 
slippery surfaces of the linerboard can cause the corners of the 
linerboard to get out of alignment and possibly tumble over, thus reducing 
the stack height of linerboard and slowing the converting operations. Wax 
adsorbed interferes with fiber-fiber bonding, which reduces product 
strength characteristics. Moreover, there is strong evidence that Scott 
bond and compression strength are reduced considerably by the presence of 
wax. 
There are three major types of wax treated boxes found in bundles of OCC: 
impregnated, saturated, and curtain-coated. They all can produce 
contamination problems because all three types can contain wax that will 
soften or melt at repulping temperatures, hindering removal and promoting 
deposition on equipment. Approaches for dealing with wax contamination 
have been threefold. The problem may be addressed upon repulping with 
improved mechanical processes to aid separation, upon application of the 
initial coating of the paper to eventually be repulped by coating 
additives; or upon improved repulping with repulping additives. This 
invention focuses on improvements of the latter type. 
Mechanical improvements to the recycling process to increase efficiency 
(the first type of solution to the problem) include the use of ultrasound 
in U.S. Pat. No. 4,045,243 and a high pressure stream of steam in U.S. 
Pat. No. 4,312,701. 
Development of more readily repulpable coatings (the second type of 
solution to the problem) that can be easily separated from fiber and 
removed with conventional cleaning systems (i.e., screens and cleaners) is 
ongoing. For example, dispersant coating additives are generally described 
in WO 91/05107. Many polymeric additives to coatings have also been 
identified. Copolymers of acrylamide/acrylic esters have been disclosed in 
U.S. Pat. No. 3,262,838; the copolymerization product of styrene and the 
half ester formed by the half esterification of 1 mole of an alpha-beta 
unsaturated dicarboxylic acid has been disclosed in U.S. Pat. No. 
3,287,149; butadiene-methyl methacrylate copolymer latex is disclosed in 
U.S. Pat. No. 4,117,199; a wax composition is disclosed in U.S. Pat. No. 
5,539,035 and a variety of other polymeric coating additives are disclosed 
in U.S. Pat. Nos. 5,491,190; 5,658,971 and 5,654,039. 
To aid the repulping process, efforts have also been focused on the 
development of more readily repulpable hot melt adhesives, as disclosed in 
U.S. Pat. No. 5,541,246 for example. 
Examples of the third type of solution, the development of repulping 
process additives include EP 0,568,229 A1 which discloses a 
hydrophobically modified associative polymer including hydrophobically 
substituted polyethylene oxide polymers; U.S. Pat. No. 4,643,800 which 
discloses use of a substituted oxyethylene glycol non-ionic surfactant and 
a water-soluble, low molecular weight polyelectrolyte dispersant; 
alkylamine polyethers for foam control disclosed in U.S. Pat. No. 
4,483,741 and U.S. Pat. No.1,628,931 which discloses use of trisodium 
phosphate. Moreover, additives to the repulping process for the removal of 
ink include long-chain alcohols as disclosed in U.S. Pat. No. 5,500,082 
and surface-active poly(ethers) in U.S. Pat. No. 4,518,459. 
Dispersion of waxes is a problem in many industrial processes, aside from 
the repulping process in the pulp and paper industry. Dissipation of waxy 
dispersions with cationic, anionic or non-ionic emulsifying agents have 
been disclosed in U.S. Pat. No. 3,537,990. Wax coagulation has been 
effected by cyanamide derivatives as disclosed in U.S. Pat. No. 4,629,477; 
by water-soluble non-ionic emulsifiers in U.S. Pat. No. 3,822,178; by a 
plant glycoside dispersion stabilizer in U.S. Pat. No. 5,403,392; by means 
of molybdenum-containing coagulants in U.S. Pat. No. 5,324,437 and by a 
mechanical technique in U.S. Pat. No. 3,940,334. 
SUMMARY OF THE INVENTION 
Methods for controlling wax and other contaminants by improving the 
dispersion of these materials through the addition of treatment agents 
such as plasticizers, dispersants or wetting agents to the process of 
recycling paper and paperboard are disclosed. Preferred treatment agents 
include polymeric wetting agents, dispersants, plasticizers and 
combinations thereof. 
DESCRIPTION OF THE INVENTION 
One aspect of this invention is a method of treating contaminants in a 
contaminated fiber slurry during recycling comprising the steps of: 
a) adding to a contaminated fiber slurry at least one plasticizer; 
b) dispersing contaminants from said contaminated fiber slurry to obtain a 
treated fiber in a contaminant-containing slurry; 
c) separating said treated fiber from said contaminant-containing slurry; 
and, 
d) recovering said treated fiber. 
Another aspect of this invention is a method of treating contaminants from 
a contaminated fiber slurry during recycling comprising the steps of: 
a) adding to a contaminated fiber slurry a composition comprising 
i) at least one hydrophobic surface active polymeric wetting agent; 
ii) at least one dispersant; 
iii) at least one plasticizer; 
b) dispersing contaminants from said contaminated fiber slurry to obtain a 
treated fiber in a contaminant-containing slurry; 
c) separating said treated fiber from said contaminant-containing slurry; 
and, 
d) recovering said treated fiber. 
Yet another aspect of this invention is a method of treating contaminants 
from a contaminated fiber slurry during a recycling process comprising the 
steps of: 
a) adding to a contaminated fiber slurry under agitation at least one 
plasticizer; 
b) dispersing contaminants from said contaminated fiber slurry to obtain a 
treated fiber in a contaminant-containing slurry; 
c) separating said treated fiber from said contaminant-containing slurry; 
and, 
d) recovering said treated fiber. 
Still another aspect of this invention is a method of treating contaminants 
from a contaminated fiber slurry during a recycling process comprising the 
steps of: 
a) adding to a contaminated fiber slurry under agitation a composition 
comprising 
i) at least one hydrophobic surface active polymeric wetting agent; 
ii) at least one dispersant; 
iii) at least one plasticizer; 
b) dispersing contaminants from said contaminated fiber slurry to obtain a 
treated fiber in a contaminant-containing slurry; 
c) separating said treated fiber from said contaminant-containing slurry; 
and, 
d) recovering said treated fiber. 
A further aspect of this invention is a method of treating contaminants 
from a contaminated fiber slurry in an aqueous repulping medium during 
repulping of old corrugated containers comprising the steps of: 
a) adding to a contaminated fiber slurry at least one plasticizer; 
b) dispersing contaminants from said contaminated fiber slurry to obtain a 
treated fiber in a contaminant-containing repulping medium; 
c) separating said treated fiber from said contaminant-containing repulping 
medium; and, 
d) recovering said treated fiber. 
Another aspect of this invention is a method of treating contaminants from 
a contaminated fiber slurry in an aqueous repulping medium during 
repulping of old corrugated containers comprising the steps of: 
a) adding to a contaminated fiber slurry a composition comprising 
i) at least one hydrophobic surface active polymeric wetting agent; 
ii) at least one dispersant; 
iii) at least one plasticizer; 
b) dispersing contaminants from said contaminated fiber slurry to obtain a 
treated fiber in a contaminant-containing repulping medium; 
c) separating said treated fiber from said contaminant-containing repulping 
medium; and, 
d) recovering said treated fiber. 
The following information may be applicable to any aspect of this 
invention. The method may further comprise the subsequent addition of a 
compound selected from the group consisting of coagulants, bentonite and 
colloidal silica. The hydrophobic surface active polymeric wetting agent 
may have an HLB value of from about 1 to about 8. More particularly, the 
hydrophobic surface active polymeric wetting agent may be an ethylene 
oxide/propylene oxide block copolymer. The dispersant may be selected from 
the group consisting of: naphthalene sulfonic acid-formaldehyde 
condensates and lignin sulfonates. Moreover, the dispersant may be a 
naphthalene sulfonic acid-formaldehyde condensate. The plasticizer may be 
selected from the group consisting of esters and ethers. More 
particularly, the plasticizer may be 2,2,4-trimethyl-1,3-pentanediol 
isobutyrate. The contaminant may be wax. One preferred treatment 
composition is an ethylene oxide/propylene oxide block copolymer, a 
naphthalene sulfonic acid-formaldehyde condensate and 
2,2,4-trimethyl-1,3-pentanediol isobutyrate. The composition may be added 
at a point in said process selected from the group consisting of: the 
repulper, the refiner and the pump. 
The additives described herein may also have utility in petroleum or 
mineral processing. Moreover, the additives could potentially have utility 
as pitch control agents, stickies and tackies removal agents, or even as 
sizing agents in the manufacture of paper. 
The Contaminants 
The contaminants to be removed may be either synthetic or natural. Among 
natural contaminants are fatty acids, rosin acids, fatty esters and 
petroleum waxes. Among synthetic contaminants are stickies, ink and 
coating binders. Stickies include contact adhesives, hot melts and 
synthetic waxes. 
The Plasticizers 
A plasticizer is anything which reduces the temperature at which a 
substance can be broken down. Several types of plasticizers are applicable 
for the practice of this invention. One type of plasticizers are adipates 
including adipic acid, dimethyl adipate, diethyl adipate, di-n-butyl 
adipate, diisobutyl adipate, di-n-hexyl adipate, di (1,3-dimethylbutyl) 
adipate, di-2-ethylhexyl adipate, diisooctyl adipate, dicapryl adipate, 
heptyl nonyl adipate, diisononyl adipate, di-n-octyl-n-decyl adipate, 
diisodecyl adipate, dicyclohexyl adipate, benzyl octyl adipate, 
dibutoxyethyl adipate, bis (2,2,4-trimethyl-1,3-pentanediol monoisobutyl) 
adipate, bis(4-chlorobutyl) adipate and diisohexyl adipate among others. 
Other types include amide-esters, azelates, benzoates, benzotriazoles, 
brassylates, carbonates, citrates, epoxy compounds, ethers, glutarates, 
glycerol esters, glycol esters, glycols, glycolates, hexahydrophthalates, 
hydrocarbons, isobutyrates, isophthalates, isosebacates, ketones, nitro 
compounds, oleates, palmitates, pentaerythritol esters, phosphates, 
phosphites, phthalates, polyesters and polymeric plasticizers, 
pyromellitates, ricinoleates, salicylates, sebacates, stearates, 
succinates, sucrose derivatives, sulfonamides, sulfonates, sulfones, 
tartrates, terephthalates, tetrahydrophthalates, thianthrenes, 
trimellitates, and terpenes and derivatives among others. 
The Wetting Agents 
For the practice of this invention, the wetting agent may be a block 
copolymer of ethylene oxide and propylene oxide. EO/PO copolymers of 
interest may have a molecular weight of from about 2000 to about 5000 and 
an EO content of from about 0 to about 30%. Preferred HLB values are from 
about 1 to about 8. Higher molecular weight structures with a low EO 
content are known as excellent wetting agents. The term "wetting agent" is 
meant to encompass agents which wet particle surfaces without raising 
energy barriers of sufficient height to disperse the particle. Examples 
may include block terpolymers which include butylene oxide/ethylene 
oxide/propylene oxide. Other examples of wetting agents which may be 
useful for the practice of this invention include polyoxyethyleneated 
alkylphenols, polyoxyethyleneated straight-chain alcohols, 
polyoxyethylenated polyoxypropylene glycols, polyoxyethylenated 
mercaptans, long-chain carboxylic acid esters, alkanolamides, tertiary 
acetylenic glycols, and polyoxyethylenated silicones among others. 
The Dispersants 
As used herein, the term dispersion refers to a process which breaks down a 
contaminant and prevents that contaminant's agglomeration and deposition 
to the point where problems associated with runnability and product 
quality are significantly reduced. A dispersant is an agent which produces 
energy barriers of sufficient height for dispersion of a particle. 
Dispersants may be ionic or non-ionic. 
A representative ionic dispersant is a naphthalene sulfonate formaldehyde 
condensed polymer. Such a polymer is available from Hampshire Chemical 
Corp. of Lexington, Mass. The naphthalene sulfonate formaldehyde condensed 
polymer has a weight average molecular weight of from about 500 to about 
120,000. Due to the chemistry involved in the formaldehyde condensation 
process, the typical polymer preparation will consist of a number of 
molecular weight species and the weight average will reflect in which 
direction the distribution of species is skewed. In no case will there be 
a single molecular weight entity and it is recognized that the 
distribution and resulting average molecular weight will be important in 
determining the efficiency of the product. In terms of intrinsic 
viscosity, IV, the anionic polymer is generally within the range of 0.02 
to 0.05, and in some instances may be as high as 0.30. 
The anionic groups are provided by naphthalene sulfonate moieties and 
control the anionic charge density of the polymer. This charge density can 
be modified by adding another condensable species, such as phenol, urea or 
melamine which will compolymerize with the naphthalene sulfonate and 
formaldehyde. In this way the charge per unit weight can be decreased by 
adding a neutral or cationic species to the cross-linked, anionic 
sulfonate. 
The charge on the anionic polymer is preferably 2.0 to 3.0 equivalents per 
kilogram but may be as low as 1.0 or as high as 4.0 equivalents per 
kilogram. 
The Treatment 
The treatments described herein will be applied at dosages tailored to the 
specific mill stream to be treated. A significant factor in determining 
how much of the treatment to utilize is the amount of wax known to be 
present in the process stream to be treated. For example, if there is from 
0-25% wax in the slurry or stream to be treated, then the treatment will 
range from 0-200 lb/ton. More particularly, if from 0-5% wax contamination 
is present, from 0-40 lb/ton of treatment may be utilized. If from 0-2% of 
wax is present in the system, the treatment level may be in the range of 
from 0-15 lb/ton. For multi-component treatments, such as those containing 
a wetting agent, a dispersant and a plasticizer, equal mass blends were 
utilized, though it is not believed that this particular ratio of the 
components is critical to activity. 
Mode of addition of the treatments to the system is not critical. The 
components (if the treatment is a multi-component one) can be pre-blended 
for addition at one point in the system, or addition at multiple points in 
the system. Moreover, each component may be fed separately to the system. 
The treatment of contaminants to decrease their interference in the 
recycling process may be accomplished in either of two ways by the 
treatments described herein. The contaminant may be sufficiently dispersed 
as to become completely dissociated from the fiber, or the contaminants 
may be retained with the fiber but in reduced size as a result of 
treatment. 
Selection of the appropriate additive, or combination of additives is 
dependant upon the type of wax contamination, the level of wax 
contamination and the temperature of the particular system to be treated. 
Mixing is advantageous to the dispersant treatment. Shear force is provided 
by the pulp and paper process itself for example from the refiners, 
repulpers, agitators, and fan pumps. Therefore agitation may be either the 
result of a specific mechanical step during the process, or may stem from 
the flow conditions inherent in the process. 
Coagulants may be used as an adjunct to the treatments described above to 
destabilize the wax dispersed by the treatments described above, for 
greater ease of removal. Coagulants useful for the practice of this 
invention include alum, polyaluminum chloride, or cationic polymers such 
as poly(amine/epichlorohydrin) condensation polymers, polyethylene imines, 
poly(aminoamide/epichlorohydrin) condensation polymers, 
poly(diallyldimethylammonium chloride), and glyoxalated 
acrylamide/diallyldimethyl ammonium chloride copolymers among others. In 
addition to coagulants other destabilizing agents such as salts or acids 
may also be adjuncts to the additives described herein. 
The following examples are presented to describe preferred embodiments and 
utilities of the invention and are not meant to limit the invention unless 
otherwise stated in the claims appended hereto.

EXAMPLE 1 
To determine the effectiveness of the treatments, the following procedure 
was utilized. Three grams of bleached kraft dry lap fiber, 250 mL of 
hardened distilled water (275.4 ppm CaCl.sub.2.2H.sub.2 O, 231 ppm 
MgSO.sub.4.7H.sub.2 O, 231 ppm NaHCO.sub.3) and the treatment chemicals 
were combined in a jacketed mixer (Eberbach Corp., Ann Arbor, Mich.) and 
allowed to equilibrate to a temperature of 125.degree. F. A sample 
(100.+-.1 mg) of crushed Amoco (Whiting, Ind.) Eskar Wax R-35, petroleum 
wax with a melting point of approximately 131.degree. F. was then added 
and the mixer was run on high for 6 minutes. The generated fiber-wax 
slurry was then filtered through a 9.0 cm Reeve Angel grade 230 paper 
filter (Whatman, Fairfield, N.J.), and the turbidity of filtrate was 
measured using a Hach Model 2100A Turbidimeter (Hach Company, Loveland, 
Colo.). Measured turbidity values for various chemical-to-wax ratios from 
the testing of several products are shown in Table 1. Background 
corrections were made for turbidity contributions from the chemistry 
alone. Higher turbidity levels correspond to higher levels of dispersion. 
Table 1 also shows results for the combination dispersants. The data 
indicates that the combination of naphthalene sulfonate and an EO/PO 
copolymer provided better performance than the individual chemistries (in 
efficiency and effectiveness in dispersing the added wax), and that the 
introduction of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate to this 
combination produced the best performance of the chemistries tested. 
TABLE 1 
__________________________________________________________________________ 
Results of Wax Dispersion Tests 
__________________________________________________________________________ 
Chemistry 0 g/g 
0.25 g/g 
0.50 g/g 
1.00 g/g 
2.00 g/g 
3.00 g/g 
4.00 g/g 
__________________________________________________________________________ 
9-10 mole % EO Ethoxylated 
43.0 
165 200 230 275 
Nonyl Phenol.sup.1 
Na Naphthalene Sulfonate.sup.2, 
45.0 
210 235 260 300 350 
MW.about.12,000, 40% Solids.sup.2 
Ammonia Lignosulfonate, 
45.0 
175 160 160 160 
Polyethylene Glycol.sup.3, 50% Solids 
Na Dioctyl Sulfosuccinate.sup.4, 
45.0 
200 260 290 300 
52.5% Solids 
2,2,4-Trimethyl-1,3-Pentanediol 
50.0 
140 132 170 170 
Diisobutyrate.sup.5 
10 mole % EO EO/PO 
30.0 
260 410 420 375 390 
Copolymer.sup.6, MW.about.3600 
Conventional Dispersant 1.sup.7 
60.0 
190 180 200 230 230 
(49% Solids) 
Conventional Dispersant 2.sup.8 
45.0 
95.0 110 140 175 
(20% Solids) 
__________________________________________________________________________ 
Chemistry (Blends) 
0 g/g 
0.20 g/g 
0.75 g/g 
1.20 g/g 
__________________________________________________________________________ 
Naphthalene Sulfonate.sup.2 (40% 
45.0 
510 465 420 
solids) and EO/PO Copolymer.sup.6 
(equal mass blend) 
Naphthalene Sulfonate.sup.2 (40% 
45.0 
490 525 650 
solids), EO/PO Copolymer.sup.6, and 
2,2,4-Trimethyl-1,3-Pentanediol 
Diisobutyrate.sup.5 (equal mass blend) 
__________________________________________________________________________ 
.sup.1 available from Nalco Chemical Co. of Naperville, IL 
.sup.2 available from Hampshire Chemical Corporation of Lexington, 
Massachusetts under the trade name DAXAD 16 
.sup.3 available from Nalco Chemical Co. of Naperville, IL 
.sup.4 available from Nalco Chemical Co. of Naperville, IL 
.sup.5 available from Nalco Chemical Co. of Naperville, IL 
.sup.6 available from Nalco Chemical Co. of Naperville, IL 
.sup.7 available from Nalco Chemical Co. of Naperville, IL 
.sup.8 available from Nalco Chemical Co. of Naperville, IL 
EXAMPLE 2 
The following method was also utilized to determine effectiveness of the 
wax dispersant treatments. Two-hundred-fifty mL of hardened distilled 
water (275.4 ppm CaCl.sub.2.2H.sub.2 O, 231 ppm MgSO.sub.4.7H.sub.2 O, 231 
ppm NaHCO.sub.3) and the treatment chemical were combined in a jacketed 
mixer (Eberbach Corp., Ann Arbor, Mich.) and allowed to equilibrate to a 
temperature of 125.degree. F. A sample of corrugated container board 
coated with petroleum wax was then added and the mixer was run for 6 
minutes. Coated board samples were produced by dipping .about.1".times.1" 
sections of board into a melted wax mixture (heated to 200.degree. F.) 
containing 20% impregnating wax and 80% saturating wax from various 
sources (Amoco, Whiting, Ind., Chevron, San Francisco, Calif., Conoco, 
Lake Charles, La., Exxon, Batton Rouge, La., Mobil, Fairfax, Va.) ranging 
in melting point from 127-150.degree. F. The coating level for these 
sections was approximately 300-400 mg per 400 mg corrugated board. The 
fiber-wax slurry generated in the mixture was then filtered through a 9.0 
cm Reeve Angel grade 230 paper filter (Whatman, Fairfield, N.J.), and a 
portion of the filtrate (100 mL) was combined with 100 mL of propanol and 
mixed for 10 minutes and passed through a preweighed 0.45 .mu.m filter 
membrane (Gelman Sciences, Ann Arbor, Mich.). The sample was then dried 
overnight and weighed. FTIR analysis indicated that the collected sample 
was composed primarily of the wax introduced to the sample. Table 3 
reports the percentage of wax added that is dispersed by the chemical as a 
function of the treatment concentration reported in g treatment per g wax. 
Results have an estimated uncertainty of .+-.7%. Dispersant A is a 
conventional wax treatment that has a solids level of approximately 20%. 
The active component is an alkoxylated alkanol amide. Dispersant B is a 
combination of an EO/PO block copolymer and naphthalene sulfonate (40% 
solids) with a solids level of 43%. Dispersant C is an equal mass 
combination of the EO/PO block copolymer, naphthalene sulfonate (40% 
solids) and 2,2,4-trimethyl-1,3-pentanediol diisobutyrate with a solids 
level of 43%. The level of wax dispersion is reported as 
##EQU1## 
The data indicates that Dispersant B greatly outperforms the conventional 
wax treatment Dispersant A. The performance of Dispersant B is then 
further increased (significantly) with the addition of 
2,2,4-trimethyl-1,3-pentanediol diisobutyrate (Dispersant C). 
TABLE 2 
______________________________________ 
Wax dispersion test results 
Conc. Conc. Conc. 
Dispersant 
wax Dispersant 
wax Dispersant 
wax 
A.sup.1 
dispersion 
B.sup.2 dispersion 
C.sup.3 dispersion 
(g/g) (%) (g/g) (%) (g/g) (%) 
______________________________________ 
0 9.7 0 11 0 11 
0.68 6.6 0.53 31 0.60 51 
1.3 7.8 1.2 44 1.2 76 
2.3 6.5 1.6 45 2.5 79 
4.9 8.5 4.6 55 4.0 84 
8.4 9.4 6.2 59 8.4 97 
9.8 9.4 8.8 62 10 97 
______________________________________ 
.sup.1 available from Nalco Chemical Co. of Naperville, IL 
.sup.2 available from Nalco Chemical Co. of Naperville, IL 
.sup.3 available from Nalco Chemical Co. of Naperville, IL 
EXAMPLE 3 
The same procedure as described in Example 2 was used with the exception of 
the temperature. Table 3 shows results at 115, 135 and 145.degree. F. The 
results indicate that increasing temperature increases the performance of 
the dispersants and that the addition of 2,2,4-trimethyl-1,3-pentanediol 
diisobutyrate to an already effective dispersant (Dispersant B) produces a 
formulation (Dispersant C) that provides greater dispersion of the wax 
both below and above its melting point. 
TABLE 3 
______________________________________ 
Wax dispersion test results at various temperatures 
Conc. Conc. Conc. 
Dispersant 
wax Dispersant 
wax Dispersant 
wax 
A.sup.1 
dispersion 
B.sup.2 dispersion 
C.sup.3 dispersion 
(g/g) (%) (g/g) (%) (g/g) (%) 
______________________________________ 
115.degree. F. 
0 1.1 0 3.0 0 2.9 
0.68 1.3 0.64 8.8 0.80 25 
1.4 1.5 1.4 11 1.4 28 
2.6 0.3 2.5 13 2.6 37 
5.9 1.8 6.8 17 6.3 40 
8.1 2.1 10 22 8.4 40 
11 1.9 12 19 12 45 
135.degree. F. 
0 9 0 11 0 11 
0.48 21 0.47 43 0.72 78 
1.1 20 1.3 69 1.1 90 
2.8 20 1.8 70 2.2 95 
3.8 19 3.7 76 4.6 100 
7.5 22 6.4 79 8.9 100 
8.6 21 7.9 76 7.5 100 
145.degree. F. 
0 17 0 18 0 17 
0.62 28 0.49 67 0.78 87 
1.1 27 1.2 70 1.3 100 
3.0 33 2.5 92 2.8 100 
4.6 35 4.6 95 5.7 100 
7.4 36 8.4 100 8.0 100 
12 39 12 93 11 100 
______________________________________ 
.sup.1 available from Nalco Chemical Co. of Naperville, IL 
.sup.2 available from Nalco Chemical Co. of Naperville, IL 
.sup.3 available from Nalco Chemical Co. of Naperville, IL 
EXAMPLE 4 
Another method to determine dispersion effectiveness is the coupon 
deposition test, described herein. A cleaned Teflon.TM. coupon was 
preweighed and fixed in the top of a jacketed mixer (Eberbach Corp., Ann 
Arbor, Mich.). Two-hundred-fifty milliliters of hardened distilled water 
(275.4 ppm CaCl.sub.2.2H.sub.2 O, 231 ppm MgSO.sub.4.7H.sub.2 O, 231 ppm 
NaHCO.sub.3) and the treatment chemical were then added and allowed to 
equilibrate to 125.degree. F. A piece of bleached kraft paper coated with 
approximately 100 mg of wax was then added, and the mixer was run for 6 
minutes. The coupon was then removed and rinsed with distilled water to 
remove any non-deposited wax, and hung up to dry. The dried weight of wax 
deposited on Teflon.TM. coupon was report as 
##EQU2## 
Tables 4 and 5 report the results of wax deposition tests at various 
temperatures on three commercially waxes used to coat corrugated 
containers. The Amoco (Whiting, Ind.) Eskar R-35 and Chevron (San 
Francisco, Calif.) Saturating Wax 2 contain paraffin wax with little or no 
additives. The Conoco (Lake Charles, La.) Supercote.TM. 4/5 is a curtain 
coating wax containing significant levels of a polymer additive. Table 4 
lists results for testing when no dispersant was added and Table 5 
presents values for when Dispersant C was added at levels of 1 g treatment 
per 1 g wax. 
The tables also show the results of dispersion tests. In that procedure 250 
mL of hardened distilled water (275.4 ppm CaCl.sub.2.2H.sub.2 O, 231 ppm 
MgSO.sub.4.7H.sub.2 O, 231 ppm NaHCO.sub.3) and the treatment chemical 
were combined in a jacketed mixer (Eberbach Corp., Ann Arbor, Mich.) and 
allowed to equilibrate to a selected temperature. A 200 mg sample of wax 
was then added and the mixer was run for 6 minutes. The fiber-wax slurry 
generated in the mixture was then filtered through a 9.0 cm Reeve Angel 
grade 230 paper filter (Whatman, Fairfield, N.J.), and a portion of the 
filtrate was used to make a turbidity measurement. Another portion (100 
mL) was combined with 100 mL of propanol and mixed for 10 minutes and 
passed through a preweighed 0.45 .mu.m filter membrane (Gelman Sciences, 
Ann Arbor, Mich.). The sample was then dried overnight and weighed. The 
level of wax dispersion is reported as 
##EQU3## 
Again, Table 4 describes performance when no dispersant was present and 
Table 5 lists dispersion results with 200 mg of Dispersant C present. The 
results indicate that for the materials composed primarily of paraffin 
waxes at a given temperature, Dispersant C is able to significantly 
improve dispersion (breaking the material down and preventing deposition). 
For materials containing higher levels of additives, Dispersant C again 
enhances dispersion. However, its greater contribution for this material 
is to prevent deposition. 
TABLE 4 
__________________________________________________________________________ 
Dispersion and deposition test results when no treatment chemical is 
present 
Chevron Saturating Wax #2 
Amoco R-35 Impregnating Wax 
Conoco 752 Curtain Coating 
% % % % % % 
Temp 
deposition 
dispersion 
Turbidity 
deposition 
dispersion 
Turbidity 
deposition 
dispersion 
Turbidity 
__________________________________________________________________________ 
80 9.3 1.0 1.0 28 1.1 1.5 9.0 2.5 0.75 
90 14 1.4 1.0 35 1.6 1.0 8.9 1.6 1.0 
100 12 2.0 1.0 41 4.6 1.0 13 2.2 1.0 
110 14 2.4 1.8 42 6.1 2.6 17 2.1 1.8 
120 12 2.4 8.0 50 0.37 44 12 1.0 1.4 
130 28 24 140 11 8.6 63 14 1.4 4.4 
140 6.4 51 250 2.2 56 350 15 4.2 25 
150 3.5 73 320 0.46 57 200 7.7 21 82 
160 3.6 69 300 1.4 75 200 5.7 19 64 
__________________________________________________________________________ 
TABLE 5 
__________________________________________________________________________ 
Dispersion and deposition test results in the presence of Dispersant C at 
a level 
of 1 mg/mg wax 
Chevron Saturating Wax #2 
Amoco R-35 Impregnating Wax 
Conoco 752 Curtain Coating 
% % % % % % 
Temp 
deposition 
dispersion 
Turbidity 
deposition 
dispersion 
Turbidity 
deposition 
dispersion 
Turbidity 
__________________________________________________________________________ 
80 3.4 2.1 9.7 3.3 1.4 8.5 2.2 1.0 10 
90 2.6 1.4 10 8.1 1.1 12 2.5 1.5 10 
100 5.4 2.2 9.8 17 2.1 9.5 2.2 3.4 9.5 
110 6.5 4.0 10 21 10 14 4.5 2.9 8.0 
120 6.5 22 58 30 46 340 8.2 2.2 10 
130 10 74 1400 9.4 81 2000 7.7 10 46 
140 1.0 83 2100 0.24 92 2400 5.5 26 340 
150 0.69 97 1900 0.0 -- 2200 0.72 55 625 
160 0.0 95 2000 0.0 100 2000 0.65 53 550 
__________________________________________________________________________ 
EXAMPLE 5 
The stability of the wax treated with this treatment was tested in the 
following manner. Five-hundred mL of hardened distilled water (275.4 ppm 
CaCl.sub.2.2H.sub.2 O, 231 ppm MgSO.sub.4.7H.sub.2 O, 231 ppm NaHCO.sub.3) 
and treatment chemical (when treatment was tested) were combined in a 2, 
250 mL, jacketed mixers (Eberbach Corp., Ann Arbor, Mich.) and allowed to 
equilibrate to a temperature of 145.degree. F. A 150 mg sample of Chevron 
(San Francisco, Calif.) Saturating Wax 2 were then added to each mixer and 
the mixer was run for 6 minutes. The wax dispersions generated were then 
combined with 2500 mL of 100.degree. F. hardened distilled water (275.4 
ppm CaCl.sub.2.2H.sub.2 O, 231 ppm MgSO.sub.4.7H.sub.2 O, 231 ppm 
NaHCO.sub.3) in a 3000 mL beaker and mixed for about 2 minutes. A 300 mL 
sample was drawn and analyzed by filtering it through a 9.0 cm Reeve Angel 
grade 230 paper filter (Whatman, Fairfield, N.J.), combining it with 200 
mL of isopropanol, mixing the sample for 10 minutes, and passing it 
through a preweighed 0.45 .mu.m filter membrane (Gelman Sciences, Ann 
Arbor, Mich.). The sample was then dried overnight and weighed. A portion 
of the remaining, untested sample, was then transferred to a 2000 mL 
Erlenmeyer flask, placed in a 100.degree. F. temperature bath, covered, 
and mixed at 500 rpm using a Britt Jar propeller (Paper Research 
Materials, Gig Harbor, Wash.). Samples were then drawn and analyzed on a 
periodic basis. Table 6 describes stability when no dispersant was 
present, and when Dispersant B and Dispersant C were present at levels of 
2 g/g wax. The results indicate that the dispersion produced with 
Dispersant C is significantly more stable than those produced with 
Dispersant B and with no dispersant present. 
TABLE 6 
______________________________________ 
Dispersion stability at 100.degree. F. 
No Dispersant Dispersant B Dispersant C 
Time Dispersion Time Dispersion 
Time Dispersion 
(hrs.) 
(%) (hrs.) (%) (hrs.) 
(%) 
______________________________________ 
0 100 0 100 0 100 
0.04 48 1 85 1 96 
0.23 31 2 87 2 102 
0.33 22 4 85 4 109 
0.42 21 8 85 8 108 
0.5 18 24 48 24 103 
1 13 -- -- -- -- 
2.2 7.3 -- -- -- -- 
______________________________________ 
EXAMPLE 6 
The treatments were also tested in the following manner. Two liters of 
hardened distilled water (275.4 ppm CaCl.sub.2.2H.sub.2 O, 231 ppm 
MgSO.sub.4.7H.sub.2 O, 231 ppm NaHCO.sub.3) were preheated to 135.degree. 
F. and added to a temperature controlled British disintegrator. One gram 
of a blend of an EO/PO copolymer, naphthalene sulfonate, and 
2,2,4-trimethyl-1,3-pentanediol diisobutyrate were added (enough to 
disperse nearly 100% of the added wax) and mixed for 30 seconds. A single 
coated board sample and 24 g of sectioned corrugated board 
(.about.1".times.1") were then added and the British disintegrator was run 
for 25 minutes (.about.77,500 revolutions). Coated board samples were 
produced by dipping .about.1".times.1" sections of board into a melted wax 
mixture (heated to 200.degree. F.) containing 20% impregnating wax and 80% 
saturating wax from various sources (Amoco, Whiting, Ind., Chevron, San 
Francisco, Calif., Conoco, Lake Charles, La., Exxon, Batton Rouge, La., 
Mobil, Fairfax, Va.) ranging in melting point from 127-150.degree. F. The 
coating level for these sections was approximately 300-400 mg per 400 mg 
corrugated board. The sample was maintained at 135.degree. F. and 250 mL 
aliquots were transferred into 400 mL plastic tri-pour beakers for 
testing. Using a Britt Jar propeller (Paper Research Materials, Gig 
Harbor, Wash.) with a mixing speed of 500 rpm, the coagulant treatment was 
mixed into the stock sample using a syringe according to the following 
mixing sequence: 
______________________________________ 
Time (seconds) Procedure 
______________________________________ 
0 start mixer 
10 add coagulant polymer 
30 stop mixer 
______________________________________ 
Immediately following this sequence the sample was filtered through Reeve 
Angel 230 paper filter (Whatman, Fairfield, N.J.), and the turbidity of 
the filtrate was measured. Results are reported as a turbidity reduction 
calculated as 
##EQU4## 
The dose (g polymer actives per g wax) necessary to achieve turbidity 
reduction values of &gt;0.80 for various coagulants is shown in Table 7. All 
treatments are conventional coagulant treatments for contaminants. This 
data indicates that once a material has been dispersed it can be removed 
(for example) through the addition of a coagulant. 
TABLE 7 
______________________________________ 
Wax Coagulant Test results. 
dose (g/g) necessary to 
achieve &gt;0.8 
Chemistry turbidity reduction 
______________________________________ 
Linear Epichlorohydrin-Dimethylamine 
0.137 
Copolymer.sup.1 
EDC/Ammonia Polymer.sup.2 
0.497 
Ammonia Crosslinked Epichlorohydrin- 
0.310 
Dimethylamine Copolymer.sup.3 
Polyacrylamide.sup.4 1.33 
Poly Diallyl Dimethylammonium Chloride 1.sup.5 
0.193 
Poly Diallyl Dimethylammonium Chloride 2.sup.6 
0.161 
Poly Diallyl Dimethylammonium Chloride 3.sup.7 
0.236 
Poly Diallyl Dimethylammonium Chloride 4.sup.8 
0.187 
______________________________________ 
.sup.1 available from Nalco Chemical Co. of Naperville, IL 
.sup.2 available from Nalco Chemical Co. of Naperville, IL 
.sup.3 available from Nalco Chemical Co. of Naperville, IL 
.sup.4 available from Nalco Chemical Co. of Naperville, IL 
.sup.5 available from Nalco Chemical Co. of Naperville, IL 
.sup.6 available from Nalco Chemical Co. of Naperville, IL 
.sup.7 available from Nalco Chemical Co. of Naperville, IL 
.sup.8 available from Nalco Chemical Co. of Naperville, IL