Abstract:
The present invention provides improved compositions and methods for producing moisture-cured adhesives and sealants based on modified silicone polymers. Methods of the present invention do not require a discrete step to dry the fillers that are incorporated into the materials and produce products with an excellent shelf life.

Description:
BACKGROUND OF THE INVENTION  
       [0001]     Modified silicone (“MS”) polymers are materials that have polypropyleneoxide as the backbone of the main chain and contain dimethoxysilyl groups that cap at end of the chains. These polymers can be formulated with various plasticizers, fillers, and other additives to produce products with specific properties to meet application requirements. The products based on MS polymers make up a wide range of high quality adhesives and sealants that may be cured under ambient conditions.  
         [0002]     One of the most desirable features of MS-based adhesives and sealants is a long shelf life. This is accomplished by producing an adhesive/sealant that has very low moisture content. Typically, the desired moisture level for such a moisture-cured adhesive/sealant should be below 0.05% or 500 ppm.  
         [0003]     The adhesives/sealants industry has traditionally used two primary methods to “dry” moisture-cured adhesives and sealants. The first is to dry all of the fillers, such as CaCO 3  and TiO 2 , in an oven, other heating device, after first grinding them to a fine powder to increase the exposed surface area. This process is generally performed under a vacuum. The other method typically used is to remove the water azeotropically by adding a solvent such as toluene to a vessel containing the fillers and removing the solvent by distillation. Both ways are very costly and time-consuming.  
         [0004]     Therefore, there remains a need to make adhesive and sealants that are less costly and time consuming. The present invention provides an improved method for the production of MS-containing adhesives and sealants that addresses the needs mentioned above as well as other objectives that will be appreciated by those skilled in the art.  
       SUMMARY OF THE INVENTION  
       [0005]     The present invention solves problems associated with the efficient production of MS polymer-based sealants and adhesives. The present invention provides methods for producing moisture-cured adhesives and sealants based on MS polymers and compositions thereof. Methods of the present invention do not require a discrete step to dry fillers that are incorporated into the materials. The present invention produces products that have a good shelf life. Additionally, the adhesives and sealants that are produced with the present invention can be free of volatile organic compounds, i.e. VOC free.  
         [0006]     Generally and in one form, the present invention provides a curable composition comprising a moisture curable material and a volatile component in an effective amount sufficient to prevent the curable composition from curing (e.g., undergoing a drying process). The weight percent of the volatile component is generally between 2% and 15%. The volatile component is one of many generally known to those of ordinary skill in the art, such as an organic solvent, an ester of a carboxylic acid, an organic acetate, a methyl ester, as examples. The curable material may further compromise a modified silicone polymer. Notably, the curable composition does not require a water-scavenging agent.  
         [0007]     The present invention also provides a method of preparing a curable composition comprising the step of combining a moisture curable material with a volatile component in an effective amount sufficient to prevent the curable composition from curing. As such, the curable material may, in one aspect, further compromise a modified silicone polymer.  
         [0008]     In yet another form, the present invention provides a curable composition comprising a moisture curable material and methyl acetate in an effective amount sufficient to prevent the curable composition from curing. The weight percent of methyl acetate is generally between 2% and 15%. When the weight percent of methyl acetate is below 2%, the non-drying process generally does not work. In addition, when the weight percent of methyl acetate is greater than 15%, the moisture-curing process is delayed at ambient temperatures. Again, the curable composition does not require a water-scavenging agent. In addition, the curable material may further compromise a modified silicone polymer.  
         [0009]     In yet another embodiment, the present invention provides a curable composition comprising a moisture curable material and a volatile component, wherein the volatile component is in an effective amount sufficient to prevent a water-scavenging agent from being required.  
         [0010]     Those skilled in the art will further appreciate the above-mentioned advantages and features of the present invention, together with other important aspects thereof upon reading the detailed description that follows in conjunction with the data provided in the tables. 
     
    
     DETAILED DESCRIPTION OF THE INVENTION  
       [0011]     Although the making and using of various embodiments of the present invention are discussed in detail below, it should be appreciated that the present invention provides a number of inventive concepts that may be embodied in a wide variety of contexts. The specific aspects of the invention discussed herein are merely illustrative of ways to make and use the present invention, and are not meant to limit its scope is any manner.  
         [0000]     Examples of Compositions and Methods of the Present Invention  
         [0012]     A general procedure is used for the preparation of compounds of the present invention in which the drying process is eliminated and a water-scavenging agent is not required. This is generally because of the addition of a volatile agent that eliminates the need for a drying process. It will be appreciated by those skilled in the art, after reading this application, that the described procedure is not the only means for achieving the results presented herein; modifications available to one of ordinary skill in the art are made to the procedure that achieve similar results. Such modifications are considered to be part of the present invention.  
         [0013]     TABLE 1 shows the process of not drying adhesives and sealants. Three samples were made in Table 1. Sample #1 was made based on a traditional process, meaning drying fillers in a mixer. An initial step for Sample #1 is the grinding of the starting materials to achieve consistence and to aid the drying process that forms one of the steps of the present invention. Typically, the polymers, fillers, pigments, UV absorbers, and thixotropic agents that are to form the basis of a composition are combined and ground to a fine paste.  
                                                                                             TABLE I                           Examples of a Non-drying Process                Sample #1   Sample #2   Sample #3            Chemical   Mass (g)   Wt %   Mass (g)   Wt %   Mass (g)   Wt %                    MS Polymer S203H   487.00   11.41   440.00   9.82   487.00   11.32       MS Polymer S303H   627.00   14.69   600.00   13.39   627.00   14.58       Winnofil SPM (CaCO3)   1412.00   33.08   1430.00   31.92   1430.00   33.25       Duramite (CaCO3)   535.00   12.54   450.00   10.04   550.00   12.79       Ti-Pure R902 (TiO2)   127.00   2.98   125.00   2.79   127.00   2.95       Aristowax 143 (Wax)   38.00   0.89   38.00   0.85   38.00   0.88       DIDP   837.00   19.61   700.00   15.63   837.00   19.46       Toluene   100.00   2.34   100.00   2.23       Methyl Acetate           500.00   11.16   100.00   2.33       Disperbyk 161   4.00   0.09   4.00   0.09   4.00   0.09       Expancel   19.00   0.45   18.00   0.40   19.00   0.44       Silquest A-171 (VTMO)   22.00   0.52   20.00   0.45   22.00   0.51       Silquest A-1120   45.00   1.05   40.00   0.89   45.00   1.05       Fomrez SUL-11A   15.00   0.35   15.00   0.33   15.00   0.35       TOTAL   4268.00   100.00   4480.00   100.00   4301.00   100.00                  
 
         [0014]     After combining the basic composition, the ground ingredients are then combined with a plasticizer and solvent, and dried. Toluene is an example of a solvent that may be used, although others may be used to azeotropically remove any water present in any of the ingredients. Before measuring the water content, the mixer is cooled down below 120 degrees Fahrenheit. With this method, it is possible to achieve moisture content as low as 0.01-0.05%, preferably 0.01-0.03%. By drying in this manner, a water-scavenging agent is not required.  
         [0015]     When all of the ingredients have been sufficiently combined, reduced pressure may once again be applied. This helps to remove any entrapped air that may be present in the finished formulation. The material may be placed in a tube, pail, or drum for eventual use in the various applications.  
         [0016]     Sample #2 and #3 are produced in a different way. Like Sample #1, Sample #2 and #3 are ground thoroughly. Instead of drying immediately after grinding, some methyl acetate is added into the formula when the mixer is below 80 degrees Fahrenheit. Following this, a dehydration agent, an adhesion promoter, a density reduction material, and a catalyst can be added into the mixer. No nitrogen protection is necessary.  
         [0017]     A stability study was conducted. Three samples stored at 120 degrees Fahrenheit for 4 weeks, were all still in a paste form without noticeable change in viscosity. As such, the concept of non-drying works. In addition, methyl acetate can block any possible curing before application. Once the non-drying adhesives and sealants are exposed to atmospheric condition, and methyl acetate is evaporated, the adhesives and sealants cured as fast as those adhesives and sealants made with drying process.  
         [0018]     More systematic study has been conducted and results indicate that the non-drying process works well to serve the stability requirement for adhesives and sealants. Better yet, the resultant products are VOC-free. TABLE 2 shows some non-drying formulas without Expancel, a density reduction material, while TABLE 3 shows some formulas with the addition of Expancel. TABLE 4 depicts results of separate sample formulas using methods of the present invention.  
         [0019]     While specific alternatives to steps of the invention have been described herein, additional alternatives not specifically disclosed but known in the art are intended to fall within the scope of the invention. Thus, it is understood that other applications of the present invention will be apparent to those skilled in the art upon reading the described embodiment and after consideration of the appended claims and drawing.  
                                                                                                                                   TABLE 2                       Non-drying Process without Expancel                                    Sample #4   Sample #5   Sample #6            Chemical   Mass (g)   Wt %   Mass (g)   Wt %   Mass (g)   Wt %               MS Polymer S203H   500.00   11.55   500.00   9.12   380.00   8.79       MS Polymer S303H   644.00   14.88   644.00   11.75   488.00   11.28       Winnofil SPM   880.00   20.33   1800.00   32.85   1360.00   31.45       (CaCO3)       Duramite (CaCO3)   1300.00   30.03   550.00   10.04   420.00   9.71       Ti-Pure R902   100.00   2.31   100.00   1.82   75.00   1.73       (TiO2)       Aristowax 143   39.00   0.90   39.00   0.71   39.00   0.90       (Wax)       diisodecyl phthatlate   689.00   15.92   860.00   15.69   650.00   15.03       Toluene   100.00   2.31   100.00   1.82   75.00   1.73       Methyl Acetate           800.00   14.60   758.00   17.53       Silquest A-171   22.00   0.51   22.00   0.40   20.00   0.46       (VTMO)       Silquest A-1120   40.00   0.92   50.00   0.91   45.00   1.04       Fomrez SUL-11A   15.00   0.35   15.00   0.27   15.00   0.35       TOTAL   4329.00   100.00   5480.00   100.0   4325.00   100.0            P/B ratio   1.99   2.14   2.14       Solid, %   98.21   84.64   86.96       Brookfield, #5   176,000   81,920   86,680       @5 rpm       Gravity, #/gallon   12.36   11.32   11.15       Channel Sag, inch   0.3   &lt;2.0   &lt;2.0       2-week Solid, %   98.01   84.21   86.30       2-week Brookfield,   181,100   84,480   87,500       #5@5 rpm       2-week Gravity,   12.28   11.39   11.14       #/gallon       2-week Channel   0.3   &lt;2.0   &lt;2.0       Sag, inch       2-week Shore A,   29   34   33       Condition       2-week Shore A,   29   34   33       QUV       4-week Solid, %   98.15   84.13   86.07       4-week Brookfield,   182,800   84,880   88,600       #5@5 rpm       4-week Gravity,   12.31   11.37   11.17       #/gallon       4-week Channel   0.3   &lt;2.0   &lt;2.0       Sag, inch       4-week Shore A,   29   34   33       Condition       4-week Shore A,   29   34   33       QUV       Tensile, psi   356.2   432.5   455.7       Elongation, %   689   678   598       Peel-Glass, pli   28.9 CF   30.2 CF   30.3 CF       Peel-Aluminum, pli   29.1 CF   29.8 CF   30.2 CF       Peel-Concrete, pli      20.1 AF/CF      18.7 AF/CF      21.6 AF/CF                        Sample #7   Sample #8            Chemical   Mass (g)   Wt %   Mass (g)   Wt %               MS Polymer S203H   380.00   9.44   380.00   9.10       MS Polymer S303H   488.00   12.12   488.00   11.69       Winnofil SPM (CaCO3)   600.00   14.91   400.00   9.58       Duramite (CaCO3)   880.00   21.86   980.00   23.47       Ti-Pure R902 (TiO2)   75.00   1.86   75.00   1.80       Aristowax 143 (Wax)   39.00   0.97   39.00   0.93       diisodecyl phthatlate   650.00   16.15   900.00   21.56       Toluene   75.00   1.86   75.00   1.80       Methyl Acetate   758.00   18.83   758.00   18.16       Silquest A-171 (VTMO)   20.00   0.50   20.00   0.48       Silquest A-1120   45.00   1.12   45.00   1.08       Fomrez SUL-11A   15.00   0.37   15.00   0.36       TOTAL   4025.00   100.00   4175.00   100.00            P/B ratio   1.79   1.68       Solid, %   87.10   83.00       Brookfield, #5 @5 rpm   65,820   7,680       Gravity, #/gallon   11.27   10.50       Channel Sag, inch   &lt;2.0   &lt;2.0       2-week Solid, %   86.25   82.19       2-week Brookfield, #5@5 rpm   67,800   8,000       2-week Gravity, #/gallon   11.25   10.51       2-week Channel Sag, inch   &lt;2.0   &lt;2.0       2-week Shore A, Condition   27   26       2-week Shore A, QUV   27   26       4-week Solid, %   85.85   82.19       4-week Brookfield, #5@5 rpm   68,200   7,900       4-week Gravity, #/gallon   11.26   10.5       4-week Channel Sag, inch   &lt;2.0   &lt;2.0       4-week Shore A, Condition   27   26       4-week Shore A, QUV   27   26       Tensile, psi   389.4   367.8       Elongation, %   723   755       Peel-Glass, pli   29.8 CF   31.2 CF       Peel-Aluminum, pli   29.4 CF   30.9 CF       Peel-Concrete, pli      17.9 AF/CF      16.9 AF/CF                  
 
         [0020]    
       
         
               
             
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
             
               
               
               
               
               
             
               
               
               
               
               
               
               
               
               
             
               
               
               
               
               
             
           
               
                 TABLE 3 
               
               
                   
               
               
                   
               
               
                 Non-drying Process with Expancel 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 Sample #9 
                   
                 Sample #10 
                   
                 Sample #11 
                   
               
             
          
           
               
                   
                 Chemical 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
               
               
                   
                   
               
               
                   
                 MS Polymer S203H 
                 487.00 
                 11.41 
                 440.00 
                 10.74 
                 440.00 
                 10.91 
               
               
                   
                 MS Polymer S303H 
                 627.00 
                 14.69 
                 600.00 
                 14.64 
                 600.00 
                 14.88 
               
               
                   
                 Winnofil SPM (CaCO3) 
                 1412.00 
                 33.08 
                 1430.00 
                 34.90 
                 1430.00 
                 35.46 
               
               
                   
                 Duramite (CaCO3) 
                 535.00 
                 12.54 
                 450.00 
                 10.98 
                 450.00 
                 11.16 
               
               
                   
                 Ti-Pure R902 (TiO2) 
                 127.00 
                 2.98 
                 125.00 
                 3.05 
                 125.00 
                 3.10 
               
               
                   
                 Aristowax 143 (Wax) 
                 38.00 
                 0.89 
                 38.00 
                 0.93 
                 38.00 
                 0.94 
               
               
                   
                 DIDP 
                 837.00 
                 19.61 
                 700.00 
                 17.09 
                 700.00 
                 17.36 
               
               
                   
                 Toluene 
                 100.00 
                 2.34 
               
               
                   
                 Water 
               
               
                   
                 Methyl Acetate 
                   
                   
                 205.00 
                 5.00 
                 141.00 
                 3.50 
               
               
                   
                 Disperbyk 161 
                 4.00 
                 0.09 
                 4.00 
                 0.10 
                 4.00 
                 0.10 
               
               
                   
                 Expancel 
                 19.00 
                 0.45 
                 20.00 
                 0.49 
                 20.00 
                 0.50 
               
               
                   
                 Silquest A-171 (VTMO) 
                 22.00 
                 0.52 
                 20.00 
                 0.49 
                 20.00 
                 0.50 
               
               
                   
                 Silquest A-1120 
                 45.00 
                 1.05 
                 50.00 
                 1.22 
                 50.00 
                 1.24 
               
               
                   
                 Fomrez SUL-11A 
                 15.00 
                 0.35 
                 15.00 
                 0.37 
                 15.00 
                 0.37 
               
               
                   
                 TOTAL 
                 4268.00 
                 100.00 
                 4097.00 
                 100.00 
                 4033.00 
                 100.00 
               
             
          
           
               
                   
                 Moisture, % 
                 0.1317 
                   
                 0.2187 
                   
               
               
                   
                 Moisture, % 
                 0.1355 
                   
                 0.2265 
               
               
                   
                 Solid, % 
                 95.02 
                   
                 95.19 
               
               
                   
                 Viscosity, Sec/20 
                 8.56 
                   
                 8.14 
               
               
                   
                 G/40 psi 
               
               
                   
                 Viscosity, Brookfield, 
                 264,300 
                   
                 264,300 
               
               
                   
                 5/5/77F 
               
               
                   
                 Gravity, #/Gallon 
                 10.58 
                   
                 10.31 
               
               
                   
                 Channel Sag, inch 
                 0 
                   
                 0.1 
               
               
                   
                 2-week Solid, % 
                 93.2 
                   
                 Cured 
               
               
                   
                 2-week Viscosity, sec/20 
                 13.18 
                   
                 In 
               
               
                   
                 G/40 psi 
               
               
                   
                 2-week Viscosity, 
                 380,000 
                   
                 Tube 
               
               
                   
                 Brookfield, 5/5/77F 
               
               
                   
                 2-week Gravity, #/gallon 
                 10.51 
               
               
                   
                 2-week Channel Sag, 
                 0 
               
               
                   
                 inch 
               
               
                   
                 2-week Shore A, 
                 32 
                   
                 33 
               
               
                   
                 condition 
               
               
                   
                 2-week Shore A, QUV 
                 32 
                   
                 33 
               
               
                   
                 4-week Solid, % 
                 94.6 
               
               
                   
                 4-week Viscosity, sec/20 
                 12.41 
                   
                 Cured 
               
               
                   
                 G/40 psi 
               
               
                   
                 4-week Viscosity, 
                 360,000 
                   
                 In 
               
               
                   
                 Brookfield, 5/5/77F 
               
               
                   
                 4-week Gravity, #/gallon 
                 10.51 
                   
                 Tube 
               
               
                   
                 4-week Channel Sag, 
                 0 
               
               
                   
                 inch 
               
               
                   
                 4-week Shore A, 
                 32 
                   
                 31 
               
               
                   
                 condition 
               
               
                   
                 4-week Shore A, QUV 
                 32 
                   
                 32 
               
               
                   
                 Tensile, psi 
                 201.1 
                   
                 178.9 
               
               
                   
                 Elongation, % 
                 345 
                   
                 374 
               
               
                   
                 100% Modulus, psi 
                 113.5 
                   
                 83.4 
               
               
                   
                 50% Modulus, psi 
                 72.8 
                   
                 46.6 
               
               
                   
                 25% Modulus, psi 
                 36.8 
                   
                 25.6 
               
               
                   
                 Peel-Glass, pli 
                 15 CF 
                   
                 10 CF 
               
               
                   
                 Peel-Aluminum, pli 
                 15 CF 
                   
                 10 CF 
               
               
                   
                 Peel-Concrete, pli 
                  7 AF 
                   
                  5 AF 
               
               
                   
                   
               
             
          
           
               
                   
                 Sample #12 
                 Sample #13 
                 Sample #14 
                 Sample #15 
               
             
          
           
               
                 Chemical 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
               
               
                   
               
               
                 MS Polymer S203H 
                 440.00 
                 10.74 
                 440.00 
                 10.73 
                 440.00 
                 10.50 
                 440.00 
                 10.51 
               
               
                 MS Polymer S303H 
                 600.00 
                 14.64 
                 600.00 
                 14.63 
                 600.00 
                 14.32 
                 600.00 
                 14.33 
               
               
                 Winnofil SPM 
                 1430.00 
                 34.90 
                 1430.00 
                 34.87 
                 1430.00 
                 34.12 
                 1430.00 
                 34.15 
               
               
                 (CaCO3) 
               
               
                 Duramite (CaCO3) 
                 450.00 
                 10.98 
                 450.00 
                 10.97 
                 450.00 
                 10.74 
                 450.00 
                 10.75 
               
               
                 Ti-Pure R902 (TiO2) 
                 125.00 
                 3.05 
                 125.00 
                 3.05 
                 125.00 
                 2.98 
                 125.00 
                 2.99 
               
               
                 Aristowax 143 (Wax) 
                 38.00 
                 0.93 
                 38.00 
                 0.93 
                 38.00 
                 0.91 
                 38.00 
                 0.91 
               
               
                 DIDP 
                 700.00 
                 17.09 
                 700.00 
                 17.07 
                 700.00 
                 16.70 
                 700.00 
                 16.72 
               
               
                 Toluene 
               
               
                 Water 
                   
                   
                 4.00 
                 0.10 
                 4.00 
                 0.10 
               
               
                 Methyl Acetate 
                 205.00 
                 5.00 
                 205.00 
                 5.00 
                 295.00 
                 7.04 
                 295.00 
                 7.05 
               
               
                 Disperbyk 161 
                 4.00 
                 0.10 
                 4.00 
                 0.10 
                 4.00 
                 0.10 
                 4.00 
                 0.10 
               
               
                 Expancel 
                 20.00 
                 0.49 
                 20.00 
                 0.49 
                 20.00 
                 0.48 
                 20.00 
                 0.48 
               
               
                 Silquest A-171 
                 20.00 
                 0.49 
                 20.00 
                 0.49 
                 20.00 
                 0.48 
                 20.00 
                 0.48 
               
               
                 (VTMO) 
               
               
                 Silquest A-1120 
                 50.00 
                 1.22 
                 50.00 
                 1.22 
                 50.00 
                 1.19 
                 50.00 
                 1.19 
               
               
                 Fomrez SUL-11A 
                 15.00 
                 0.37 
                 15.00 
                 0.37 
                 15.00 
                 0.36 
                 15.00 
                 0.36 
               
               
                 TOTAL 
                 4097.00 
                 100.00 
                 4101.00 
                 100.00 
                 4191.00 
                 100.00 
                 4187.00 
                 100.00 
               
             
          
           
               
                 Moisture, % 
                 0.08418 
                 0.2269 
                 0.2761 
                 0.1121 
               
               
                 Moisture, % 
                 0.07411 
                 0.2472 
                 0.2923 
                 0.1326 
               
               
                 Solid, % 
                 95.67 
                 97.82 
                 95.7 
                 96.57 
               
               
                 Viscosity, sec/20 
                 8.67 
                 22.84 
                 14.39 
                 16.04 
               
               
                 G/40 psi 
               
               
                 Viscosity, Brookfield, 
                   
                 188,800 
                 256,000 
                 325,100 
               
               
                 5/5/77F 
               
               
                 Gravity, #/gallon 
                 10.53 
                 10.51 
                 10.35 
                 10.37 
               
               
                 Channel Sag, inch 
                 0.1 
                 0.05 
                 &gt;0.3 
                 0 
               
               
                 2-week Solid, % 
                 95.43 
                 98.02 
                 Cured 
                 95.67 
               
               
                 2-week Viscosity, 
                 27.98 
                 128.52 
                 In 
                 20.91 
               
               
                 sec/20 G/40 psi 
               
               
                 2-week Viscosity, 
                 289,900 
                 239,000 
                 Tube 
                 313,200 
               
               
                 Brookfield, 5/5/77F 
               
               
                 2-week Gravity, 
                 10.52 
                 10.49 
                   
                 10.34 
               
               
                 #/gallon 
               
               
                 2-week Channel Sag, 
                 0.1 
                 0 
                   
                 0 
               
               
                 inch 
               
               
                 2-week Shore A, 
                 32 
                 33 
                   
                 30 
               
               
                 condition 
               
               
                 2-week Shore A, 
                 32 
                 33 
                   
                 30 
               
               
                 QUV 
               
               
                 4-week Solid, % 
                 95.23 
                 87.34 
                   
                 95.52 
               
               
                 4-week Viscosity, 
                 24.73 
                 223.1 
                 Cured 
                 31.1 
               
               
                 sec/20 G/40 psi 
               
               
                 4-week Viscosity, 
                 295000 
                 320,000 
                 In 
                 357,700 
               
               
                 Brookfield, 5/5/77F 
               
               
                 4-week Gravity, 
                 10.53 
                 10.54 
                 Tube 
                 10.44 
               
               
                 #/gallon 
               
               
                 4-week Channel Sag, 
                 0 
                 0 
                   
                 0 
               
               
                 inch 
               
               
                 4-week Shore A, 
                 31 
                 32 
                 32 
                 30 
               
               
                 Condition 
               
               
                 4-week Shore A, 
                 30 
                 31 
                 32 
                 30 
               
               
                 QUV 
               
               
                 Tensile, psi 
                 181.5 
                 185.9 
                 176.5 
                 179.2 
               
               
                 Elongation, % 
                 380 
                 383 
                 390 
                 361 
               
               
                 100% Modulus, psi 
                 75.2 
                 78.5 
                 68.5 
                 47.4 
               
               
                 50% Modulus, psi 
                 50.1 
                 47.3 
                 48.9 
                 24.2 
               
               
                 25% Modulus, psi 
                 27.5 
                 24.6 
                 26.3 
                 12.2 
               
               
                 Peel-Glass, pli 
                 10 CF 
                 10 CF 
                 10 CF 
                 10 CF 
               
               
                 Peel-Aluminum, pli 
                 10 CF 
                 10 CF 
                 10 CF 
                 10 CF 
               
               
                 Peel-Concrete, pli 
                 5.5 AF  
                  5 AF 
                  6 AF 
                  4 AF 
               
               
                   
               
             
          
         
       
     
         [0021]    
       
         
               
             
               
               
               
               
             
               
               
               
               
               
               
               
             
               
               
               
               
             
               
               
               
               
             
               
               
               
               
               
               
               
             
               
               
               
               
             
           
               
                 TABLE 4 
               
               
                   
               
               
                   
               
               
                 Additional Sample Batches with a Non-drying Process 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 Sample #16 
                 Sample #17 
                 Sample #18 
               
             
          
           
               
                 Chemical 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
               
               
                   
               
               
                 MS Polymer S203H 
                 370 
                 10.67 
                 370 
                 10.55 
                 370 
                 10.55 
               
               
                 MS Polymer S303H 
                 476 
                 13.72 
                 476 
                 13.57 
                 476 
                 13.57 
               
               
                 Neolight (CaCO3) 
                 1100 
                 31.71 
                 1100 
                 31.37 
                 1100 
                 31.37 
               
               
                 Duramite (CaCO3) 
                 400 
                 11.53 
                 400 
                 11.41 
                 400 
                 11.41 
               
               
                 Ti-Pure R902 (TiO2) 
                 96 
                 2.77 
                 96 
                 2.74 
                 96 
                 2.74 
               
               
                 Aristowax 143 (Wax) 
                 28 
                 0.81 
                 28 
                 0.80 
                 28 
                 0.80 
               
               
                 Jayflex DIDP 
                 635 
                 18.30 
                 635 
                 18.11 
                 635 
                 18.11 
               
               
                 Disparlon 6500 
               
               
                 CaO 
                 32 
                 0.92 
                 70 
                 2.00 
                 70 
                 2.00 
               
               
                 Methyl Acetate 
                 240 
                 6.92 
                 240 
                 6.84 
                 240 
                 6.84 
               
               
                 Disperbyk 161 
                 3 
                 0.09 
                 3 
                 0.09 
                 3 
                 0.09 
               
               
                 Expancel 
                 16 
                 0.46 
                 16 
                 0.46 
                 16 
                 0.46 
               
               
                 Silquest A-171 (VTMO) 
                 17 
                 0.49 
                 17 
                 0.48 
                 17 
                 0.48 
               
               
                 Silquest A-1120 
                 44 
                 1.27 
                 44 
                 1.25 
                 44 
                 1.25 
               
               
                 Fomrez SUL-11A 
                 12 
                 0.35 
                 12 
                 0.34 
                 12 
                 0.34 
               
               
                 TOTAL 
                 3469 
                 100.00 
                 3507 
                 100.00 
                 3507 
                 100.00 
               
             
          
           
               
                 Moisture, % 
                 0.1743 
                 0.2003 
                 0.1643 
               
               
                 Before CaO 
                 0.1809 
                 0.2043 
                 0.1770 
               
               
                 Moisture, % 
                 0.1759 
                 0.1586 
                 0.1555 
               
               
                 After CaO 
                 0.1875 
                 0.1720 
                 0.1440 
               
               
                 Solid, % 
                 96.46 
                 97.02 
                 96.39 
               
               
                 Viscosity, Sec/20 G/40 psi 
                 11.82 
                 8.46 
                 9.53 
               
               
                 Viscosity, Sec/20 G/60 psi 
               
               
                 Viscosity, Brookfield, 
                 358,400 
                 320,600 
                 348,800 
               
               
                 5/5/77F 
               
               
                 Viscosity, Brookfield, 
               
               
                 7/100/77F 
               
               
                 Gravity, #/Gallon 
                 10.20 
                 10.22 
                 10.20 
               
               
                 Channel Sag, inch 
                 0.00 
                 0.00 
                 0.00 
               
               
                 2-week Solid, % 
                 97.03 
                 96.78 
                 96.45 
               
               
                 2-week Viscosity, sec/20 
                 29.31 
                 22.63 
                 24.52 
               
               
                 G/40 psi 
               
               
                 2-week Viscosity, sec/20 
               
               
                 G/60 psi 
               
               
                 2-week Viscosity, 
                 555,500 
                 503,400 
                 551,000 
               
               
                 Brookfield, 5/5/77F 
               
               
                 2-week Viscosity, 
               
               
                 Brookfield, 7/100/77F 
               
               
                 2-week Gravity, #/gallon 
                 10.21 
                 10.20 
                 10.21 
               
               
                 2-week Channel Sag, inch 
                 0.00 
                 0.00 
                 0.00 
               
               
                 2-week Shore A, Condition 
                 32 
                 32 
                 33 
               
               
                 2-week Shore A, QUV 
                 33 
                 33 
                 32 
               
               
                 4-week Solid, % 
                 97.41 
                 97.02 
                 96.65 
               
               
                 4-week Viscosity, sec/20 
                 36.56 
                 24.81 
                 43.15 
               
               
                 G/40 psi 
               
               
                 4-week Viscosity, sec/20 
               
               
                 G/60 psi 
               
               
                 4-week Viscosity, 
                 98,800 
                 96,000 
                 145,000 
               
               
                 Brookfield, 7/100/77F 
               
               
                 4-week Gravity, #/gallon 
                 10.22 
                 10.23 
                 10.2 
               
               
                 4-week Channel Sag, inch 
                 0 
                 0 
                 0 
               
               
                 4-week Shore A, condition 
                 33 
                 33 
                 33 
               
               
                 4-week Shore A, QUV 
                 32 
                 33 
                 33 
               
               
                 Tensile, psi 
                 160.7 
                 161.1 
                 158.3 
               
               
                 Elongation, % 
                 360 
                 380 
                 374 
               
               
                 100% Modulus, psi 
                 76.4 
                 78.4 
                 72 
               
               
                 50% Modulus, psi 
                 49.1 
                 48.8 
                 46.5 
               
               
                 25% Modulus, psi 
                 28.8 
                 29.3 
                 29.2 
               
               
                 Peel-Glass, pli 
                 10.2 CF 
                 10 CF 
                 10 CF 
               
               
                 Peel-Aluminum, pli 
                 10.6 CF 
                 10 CF 
                 10 CF 
               
               
                 Peel-Concrete, pli 
                   7 AF 
                  7 AF 
                     8 AF/CF 
               
               
                   
               
             
          
           
               
                   
                 Sample #19 
                 Sample #20 
                 Sample #21 
               
             
          
           
               
                 Chemical 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
                 Mass (g) 
                 Wt % 
               
               
                   
               
               
                 MS Polymer S203H 
                 370 
                 11.57 
                 335 
                 10.08 
                 335 
                 9.87 
               
               
                 MS Polymer S303H 
                 476 
                 14.88 
                 428 
                 12.88 
                 428 
                 12.61 
               
               
                 Neolight (CaCO3) 
                 1100 
                 34.39 
                 1430 
                 43.02 
                 1430 
                 42.13 
               
               
                 Duramite (CaCO3) 
                 200 
                 6.25 
               
               
                 Ti-Pure R902 (TiO2) 
                 96 
                 3.00 
                 200 
                 6.02 
                 300 
                 8.84 
               
               
                 Aristowax 143 (Wax) 
                 28 
                 0.88 
                 25 
                 0.75 
                 25 
                 0.74 
               
               
                 Jayflex DIDP 
                 550 
                 17.19 
                 500 
                 15.04 
                 450 
                 13.26 
               
               
                 Disparlon 6500 
                   
                   
                 45 
                 1.35 
                 45 
                 1.33 
               
               
                 CaO 
                 64 
                 2.00 
                 60 
                 1.81 
                 60 
                 1.77 
               
               
                 Methyl Acetate 
                 230 
                 7.19 
                 220 
                 6.62 
                 240 
                 7.07 
               
               
                 Disperbyk 161 
                 3 
                 0.09 
                 2 
                 0.06 
                 2 
                 0.06 
               
               
                 Expancel 
                 15 
                 0.47 
                 14 
                 0.42 
                 14 
                 0.41 
               
               
                 Silquest A-171 (VTMO) 
                 15 
                 0.47 
                 14 
                 0.42 
                 14 
                 0.41 
               
               
                 Silquest A-1120 
                 40 
                 1.25 
                 40 
                 1.20 
                 40 
                 1.18 
               
               
                 Fomrez SUL-11A 
                 12 
                 0.38 
                 11 
                 0.33 
                 11 
                 0.32 
               
               
                 TOTAL 
                 3199 
                 100.00 
                 3324 
                 100.00 
                 3394 
                 100.00 
               
             
          
           
               
                 Moisture, % 
                 0.1950 
                 0.2067 
                 0.1703 
               
               
                 Before CaO 
                 0.2049 
                 0.1922 
                 0.1712 
               
               
                 Moisture, % 
                 0.1798 
                 0.1653 
                 0.1554 
               
               
                 After CaO 
                 0.1881 
                 0.1573 
                 0.1636 
               
               
                 Solid, % 
                 97 
                 93.12 
                 92.45 
               
               
                 Viscosity, Sec/20 G/40 psi 
                 10.37 
               
               
                 Viscosity, Sec/20 G/60 psi 
                   
                 10.23 
                 6.17 
               
               
                 Viscosity, Brookfield, 
                 402,800 
               
               
                 5/5/77F 
               
               
                 Viscosity, Brookfield, 
                   
                 130000 
                 110000 
               
               
                 7/100/77F 
               
               
                 Gravity, #/gallon 
                 10.11 
                 10.7 
                 10.8 
               
               
                 Channel Sag, inch 
                 0.00 
                 0 
                 0 
               
               
                 2-week Solid, % 
                 96.87 
                 95.48 
                 94.53 
               
               
                 2-week Viscosity, sec/20 
                 28.3 
               
               
                 G/40 psi 
               
               
                 2-week Viscosity, sec/20 
                   
                 27.49 
                 11.64 
               
               
                 G/60 psi 
               
               
                 2-week Viscosity, 
                 610,000 
               
               
                 Brookfield, 5/5/77F 
               
               
                 2-week Viscosity, 
                   
                 185,600 
                 148,100 
               
               
                 Brookfield, 7/100/77F 
               
               
                 2-week Gravity, #/gallon 
                 10.12 
                 10.75 
                 10.85 
               
               
                 2-week Channel Sag, inch 
                 0.00 
                 0.00 
                 0.00 
               
               
                 2-week Shore A, condition 
                 32 
                 37 
                 36 
               
               
                 2-week Shore A, QUV 
                 33 
                 36 
                 36 
               
               
                 4-week Solid, % 
                 97.04 
                 95.57 
                 93.44 
               
               
                 4-week Viscosity, sec/20 
                 30.84 
               
               
                 G/40 psi 
               
               
                 4-week Viscosity, sec/20 
                   
                 37.74 
                 12.67 
               
               
                 G/60 psi 
               
               
                 4-week Viscosity, 
                 103,300 
                 220,100 
                 155,500 
               
               
                 Brookfield, 7/100/77F 
               
               
                 4-week Gravity, #/gallon 
                 10.14 
                 10.58 
                 10.95 
               
               
                 4-week Channel Sag, inch 
                 0 
                 0 
                 0 
               
               
                 4-week Shore A, condition 
                 32 
                 36 
                 37 
               
               
                 4-week Shore A, QUV 
                 32 
                 37 
                 36 
               
               
                 Tensile, psi 
                 173.6 
                 167.9 
                 165.5 
               
               
                 Elongation, % 
                 392 
                 342 
                 359 
               
               
                 100% Modulus, psi 
                 82.6 
                 86.9 
                 84.5 
               
               
                 50% Modulus, psi 
                 52.1 
                 53.2 
                 56 
               
               
                 25% Modulus, psi 
                 31.2 
                 33.2 
                 37.5 
               
               
                 Peel-Glass, pli 
                 10.5 CF 
                 12.2 CF 
                 13.8 CF 
               
               
                 Peel-Aluminum, pli 
                 10.5 CF 
                 11.7 CF 
                 14.2 CF 
               
               
                 Peel-Concrete, pli 
                     8.5 AF/CF 
                  7.2 AF 
                  6. AF