Document em8NzBOOLQQ6L4ZBeN9n8VV0M
BUSINESS CONFIDENTIAL.
PLAINTIFFS EXHIBIT
UC-867
iEC" REPORT
WEATHER-BARRIER MASTICS IMPROVED PERFORMANCE WITH AN EXPERIMENTAL ACRYLIC LATEX MIXTURE IN THE FORMULATION
authors:
d. H. Reed
supervisor: Dr. R. Stickle, Jr.
date:
September 8, 1969
PROJECT NO.: 322123
file no.:
12576
SUMMARY A mastic formulation has been developed based on a mixture of UCAR Latex 874 KS (90.3%) and BAKELITE
Aqueous Ink Resin M-3 (9.7%). The new mastic passes the shrinkage tests, elongation and low temperature requirements for an acrylic mastic. Exposure performance has not been established as yet.
The most striking feature of the new mastic, compared to product based on UCAR Latex 891, is much improved adhesion to glass, ceramic tile, aluminum, steel and wood. In addition there is reason to believe the new latex will minimize some of the settling and foaming problems which have plagued UCAR 891.
INTRODUCTION The investigation of a new latex for weatherbarrier mastic formulation application was started
for two reasons. One, there has been a recurring question about the product stability of UCAR Latex 891 by one of our customers, B and B Engineering, of Houston, Texas. Secondly, Mr. Herb Rosenblatt, Technical Director of Desota, Inc., Sonneborn Division DesPiaines, Illinois, expressed interest to Mr. Frank Squillaro, Carbide Salesman, for a mastic that had good adhesion to wood and steel substrates and have a certain degree of flame retardancy (1)
Messrs. W. F. Hill, Jr., of this Department, and C. E. Metten, now in the Sales Department, developed the UCAR 891, E-1166, basic mastic formulation. The basic formulation is a good one. However, it did not meet The basic adhesion require ments of Mr. Rosenblatt and was difficult to formulate with UCAR 891. Attempts to get adhesion with UCAR 891 and Silane Adhesion Promoter A-187 were successful; however, prolonged mastic storage resulted in an unstable mastic.
RESEARCH AND DEVELOPMENT DEPARTMENT CHEMICALS AND PLASTICS
UNION CARBIDE CORPORATION SOUTH CHARLESTON, WEST VIRGINIA
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BUSINESS CONFIDENTIAL 322123
2
DISCUSSION The performance of UCAR Latex 891 in mastic formulat
ing has oeen somewhat spotty, according to Mr. Joe
Venable of B and B Engineering. On a recent visit with Mr. Venable,
he indicated a strong desire for a more stable latex for this
application. Coincidental with Mr. Venable's problem was the
request from Mr. Rosenblatt for a mastic with good adhesion proper
ties. Work was already ir. progress on the use of BAKELITE
Aqueous Dispersion M-3 Qethyiene/20% acrylic acid copolymer in
dimethylethanolamine and water (32.5%
, as an adhesion pro
moter in UCAR Latex 874 KS (58% S).
The mixture of UCAR 874 and M-3 resins gives a clear film which is softer than either resin. For example, the Sward Hardness of a 0.008 inch cured film of UCAR Latex 874 v/as 4, the M-3 was 3, and a 96%/4% M-3 mixture reading was 1. A qualitative observation under the microscope also indicates that the mixture has a softer film than either latex cured singly. Both latexes are softened by FLEXOL Plasticizers TBF and tricresyl phosphate. The latex mixture, used in the E-1166 mastic formulation, con sisted of 90.3% by weight UCAR Latex 874 HS (58% s') and 9.3% M-3 (32.5% S'). The mixture contains about 55.5% s'. The shelf stability of the mixture is still good at 2 1/2 months. There are no apparent seeds, separation, or viscosity build-up.
Tne only other change made in the E-1166 nasic formu lation was to use Calidria SG-210 Grade asbestos. The original formulation suggested asbestos 7M (40 parts) and 5K (20 parts). The latter is a long fiber type asbestos.
Basic Formulation (12-DHR-50) and Estimated RMC
The basic mastic formulation is listed in attached Table I. The formulation has a higher total solids content than the former E-1166 (71% versus 64) and a subsequent slightly
higher density (10.5 versus 10.42 Ibs/gal). In calculating the estimated RMC, 80 cents/dry pound was used for the M-3 resin. This, along with the higher , increased the estimated RMC from $1.40/gallon to $1.65/gallon. As a note of interest, the latter cost is in the range of a low quality butyl rubber caulk.
The mastic mixing procedure, using UCAR 891 Latex, was quite critical with respect to excess foam, aeration, and mastic viscosity stability. In the suggested mixing procedure for (12-DHR-50), Table II, the only ingredient that might take a little extra time to wet is asbestos. This caution is needed to minimize lumping. In general, foam has not been a problem. The final formulation is certainly not air-free; however, air has not posed a problem in the formulations made to date (3 one-gallon batches).
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BUSINESS CONFIDENTIAL 322123
Tensile, Elongation Test Data
The weather-barrier mastic (12-DHR-50), was tested by the tentative lest procedures shown m attached Appendix A. The tensile and elongation delta are listed in Table III. These data were obtained by Mr. D. II. Mullin, or this Department. A comparison of the average results with those of -1166(3) and a commercial material, from the Napco Corporation, Houston, Texas, are depicted in Table VI. The data are those representating accelerated aging cure. The most notable differences are in the % elongation values. As expected, the tensile strength, psi, decreased somewhat. This usually happens when the film elongation increases, particularly when the only change is in additives.
In general, the new latex mixture increased elongation from about 45 to 200%. The Napco material has very little elongation. As a result, it has a significantly higher tensile strength. The Napco mastic film extensibility is such that shrinkage cracks might present a problem.
180 Peel Adhesion N Perhaps the most important data, as far as Desoto is
concerned, are the 180 Peel Adhesion results. These data are listed in Table IV. Corresponding data on the UCAR 891 Latex and Napco materials are shown in Table VII. These data show that the adhesion properties of the cured films increase from 0.5 p.i. to about 22 p.i. on difficult to bond substrates. In addition, test number 11, Table IV, shows that, with incomplete drying, see Figure 1, on a porous substrate (pinewood), complete rewetting (submersion in water), and on redrying there is still excellent adhesion. The bond to glass, aluminum, steel, wood, and ceramic tile are such that cohesive film failure is obtained. In contrast, E-1166 and Napco materials show adhesive film failures, under the same test conditions, Appendix A. These results represent a tremendous improvement over the UCAR 891 Latex mastics.
Miscellaneous Test Data
There were certain miscellaneous tests performed on the material that are pertinent to end-use applications. These data are listed in Table V, and pertain to the film hardness, slump, temperature sensitivity, shrinkage, and viscosity stability. Also included is the drying rate on a non-porous substrate, at room temperature, Figure 1.
The (12-DHR-50) mastic is softer than the E-1166 formula tion with UCAR 891 Latex. It has a Shore A Hardness of 23.6, as opposed to about 75 for E-1166. This will probably make it more subject to dirt pickup. The material does not slump, shrink from the lips of a filled aluminum cup, has very little viscosity buildup under accelerated temperature conditions, and the cured film is flexible at -15C.
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BUSINESS CONFIDENTIAL
322123
4
It should also be noted, in Figure 1, that on a nonporous substrate, the removal of the last traces of water is quite slow. The theoretical water content is 2S.9% by weight. About 9% water still remained in the 1/16-inch film after 23 hours. However, the surface cure of the applied film is such that it is not attacked by running top-water, after about 2 hours, Figure 1. This was determined by casting a (6X.025 inch) film on glass and checking water sensitivity at various time intervals. At two hours cure, at (77F-50% R.H.), the film appeared impervious to tap-water, even under pressure. This means that rain-water should not be a problem if it occurs a couple of hours after application.
BIBLIOGRAPHY
(1) D. Harold Reed, Letter to Mr. Frank Squillaro, Clifton Sales Office, May 12, 1969.
(2) D. Harold Reed, Letter to Mr. R. M. Nilson, Chicago Sales Office, August 15, 1969.
(3) C. E. Metten, Letter to Mr. J. Nesmith, New York Office, 33rd Floo \ February 26, 1969.
NOTEBOOK REFERENCE: 12-DHR-50
Attachments 7 Ta b1 es 1 Figure 1 Appendix A
D. Harold Reed
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rr\ -- -- -- a
WEATHER BARRIER MASTIC (I2-DBR-50)
Ingredients
Pounds
1. Experimental UCAR Latex,
2434.8
Union Carbide (55.5% j)
2. Pigment Paste Dispersion
. 3.6
Super Imperse Blue B (50% g)
3. Calgon
11.2
4. Calidria SG-210 Asbestos,
44.0
Union Carbide
5. Mica, Mineralite 3X
508.8
6. Titanium Dioxide (R-901)
35.2
7. Clay, Kingsley
169.2
S. Chiorowax 70 9. Antimony Oxide
79.2
6.0
10. s Dicalite SA-3
248.4
11. Tricresyl Phosphate, Union Carbide 223.6
12. PiIA-30
8.0
13. Colloid 581B (15% *g)
9.6
3781.6
Pounds/ 100 Gallons
681.89
1.01
3.14 12.22
142.48 9.85
47.39 22.19
1.71 69.57 62.62
2.23 2.70
1059.00
% by V."
64.39
0.10
0.30 1.16
13.45 0.93 4.47 2.09 0.15
5.53 5. Si
0.21 0.25
100.00
Total Solids, % by \vt Density, Ibs/gallon Estimated RMC, $/gallon
71.1 10.59 1.65
& 2 3 32 7
TAEnE il
WEATHER BARRIER MASTIC (12-DER-50) SUGGESTED MIXING PROCEDURE
Ingredients and Order of Addition
1. Experimental UCAR Latex 2. Pigment Paste Dispersion, Super Imperse Blue B (50% S' 3. Caigon
Note: Mix until homogeneous 4. Calidria SG-210 Asbestos
Note: Mix until lumps have disappeared, or until the asbestos is thoroughly wet. Add Singly or as a Mixture
5. iiics. t Mxreralite 3X 6. iiL Jl. *C2. .L Vilil Dioxide (R-901) 7.N Kingsley Clay S. Chlorowax 70 9. Antimony Oxide 10. Dicalite SA-3
Note: Mix until the particles are wetted. 11. Tricresyl Phosphate 12. PMA-30 13. Colloid 581B
Mixing: The above mixture is then mixed for two hours in a one-gallon Baker-Perkins, Sigma Blade Type Mixe at 79 rpm. A plant-size mixer, in most cases, is more efficient.
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TAELS III
TENSILE DATA WEATHER BARRIER MASTIC (12- DHR-50)
Film Cur ed 1/2
Tests Run at Room Temner ature
Tensile , psi
% Siong at ion
Ereak Yield
Break Yield
Hour at 1 50 ?
Tests Run
Tensile, psi
Ereak
Yield
^A jlm oOv~ 0 --*^ % Siong cion Yield
33 38 44 39 43 30 Avg.38
0 68 66 . 77 66 6S 71
314 261 147 216 264 308 252
64 299
>200 (a)
69
205
-
>200 (a)
-
70
232
-
>200 (a)
-
64 310 - 120 -
85 Avg. 261
Appr ox.200
70
70
Note: (a) Non
, IT eached
limits of extensibility in
environmental chamber.
X
Film Cured at Ecu rs/F:
Tests Run at Room Temoera
Tensil e, psi
% Elonga tier.
Break Yield
Break Yield
189 162 177 202 1SS 203 164 108 ;. 172
'
201 163 203 206 177 207 166 115 180
219 218 226
200 277 229 259 222 231
164 213 166
170 210 200 203 150 185
0.5/150 + 0.5/225 +
Tests Run Tensi!i.e, psa Ereak : Yield
-- Cf / ouO
_ .aa c
oo
er
u
o
--r^
-
% Siong ation
lx Yield
491 575 630 444 395 217 245 213
401
mm 173
- 183 - 144 - >200(a) - 143 - >200 (a) - >200(a) - >200(a)
Approx.200
-
4?3
29
WEATHER BARRIER MASTIC (12-DHR-50) TENSILE ADHESION DATA, 180 PEEL TEST (b)
Films Cured 3 Days at 77F - 50% Relative Humidity
Tensile, p.i.
Type of Failure
1. 180 Peel, Adhesion to yellow pine wood 19.0 (a)
2. 180 Peel, Adhesion to aluminum
18.5 (a)
Cohesive Cohesive
3. 180. Peel, Adhesion to steel
19.0 (a)
Cohesive
4. 180 Peel, Adhesion to glass
15.4 (a)
Cohesive, trace of adhesive
5. 180 Peel, Adhesion to ceramic tile
19.0 (a)
Cohesive, trace of adhesive
Films; Cured Overnight at 60C, Recondlition to 77F - 50% R. H.
6. 180 Peel, Adhesion to aluminum
20.53 (a)
7. 180 Peel, Adhesion to steel
21.30 (a)
8. 1S0 Peel, Adhesion to glass
22.00 (a)
9. 180 Peel, Adhesion to ceramic tile
22.00 (a)
.0. 180 Peel, Adhesion to yellow pine v/ood 22.00 (a)
LI. 180 Peel, Adhesion to yellow pine wood 26.5
Cohesive Cohesive Cohesive Cohesive Cohesive Cohesive (c)
Note:
(a) The films were pulled to maximum extensibility and then cut with a razor blade to get the average p.i. over a (6" x 1") area.
(b) See Test Procedure.
(c) The film was cured overnight at 77F-50% R.H., submerged 24 hours in water, cured 4 days at 77F-50% R.H., and then tested.
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'T* * rtr t> V
* A* XJXJ Xj V
WEATHER BARRIER MASTIC (I2-DHR-50) ADDITIONAL PROPERTIES
1. Shore A Hardness (5" x 2" x 1/4") Film on Aluminum
23.6
2. Film Flexibility (6" x 1" x 0.025") Film on Teflon:
(a) At -20C becomes hard
(b) At -15C will wrap around a 1/2" diameter preconditioned aluminum rod.
3. Viscosity Stability
N (a) At 23C 101 grams through a 1/S" orifice, under 50 psi pressure in a 6-oz polyethylene caulk cartridge, in 10 seconds.
(b) After 20 days in 60C oven, 113 grams under the same condition.
'4. Slump in a 6" x 3/4" width x 1/2" depth steel channel - None
5. Aluminum cup shrinkage - No cracking or pulling away from the lips of the cup.
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TABLE VI
TENSILE PROPERTIES
COMPARISON OF COMMERCIAL AND "UCAR" 891 MASTICS WITH (12-DHR-50)
u
TEST TEMPERATURE
(12-DHR-50)
Room Temperature
Tensile >
%
psi Elongation
172
231
35F
Tensile,i
C/of
psi
Elongation
401
Approx.200
UCAR 891 (E-1166)a
483
44
819
59
NAPCO Mastic, S-230S, Napco Corporation, Houston, Texas
N
600
19
1870
4
Note:
aLetter by Mr. C. E. Metten to Mr. J. Nesmith, February 26, 1969.
DTiie above films were cured 0.5 hours at 150F plus 0.5 hours at 225F plus 1.5 hours at 300F to simulate aged conditions. The Instron data were obtained by Mr. D. H. Mullins.
CNon-breaks, four of the eight test films reached limits of extensibility in the environmental chamber.
A 2 3.3
TABLE VII
WEATHER BARRIER MASTICS TENSILE ADHESION DATA, 180 PEEL TEST FILMS CURED 3 DAYS AT 77F - 50% RELATIVE HUMIDITY
UCAR 891 Mastic Formulation B-1166
Tensile,
n. i.
1. 180 Peel, Adhesion to steel
3.6
2. 1S0 Peel, Adhesion to aluminum
1.0
3. N 180 Peel, Adhesion to glass
1.5
4. 180 Peel, Adhesion to yellow pine wood 2.0
Type of Failure
Adhesive trace of cohesive
Adhesive
Adhesive
Adhesive
Napco, A Commercial Mastic
5. 180 Peel, Adhesion to steel
2.0
6. 180 Peel, Adhesion to aluminum
0.5
7. 1S0 Peel, Adhesion to glass
*
3.0
8. 180 Peel, Adhesion to yellow pine wood 4.5
Adhesive Adhesive Adhesive Adhesive
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RESEARCH AND DEVELOPMENT
FIGURE 1
DRYING RATE WEATHER-BARRIER MASTIC (22-DKR-50)
% Water Vs Time 1/16 Inch Layer in a Concentric Plastic Disc
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