Document jmNj5NR18nbbVMxbKQ8jMyeeN

NSW ADDITIVES INDUCE THIXOTROFY, PROVIDE SAG AND VISCOSITY CONTROL John. L. Myers Technics! Superintendent Reprint of paper presented in May 1969 to the Western Coatings Technology Society Meetings in Denver, Los Angeles, San Francisco, Portland, Seattle, and Vancouver, B. C. PLAINTIFF'S | EXHIBIT I 7 Ud-,1484 ? : NEW ADDITIVES INDUCE THIXOTROPY, PROVIDE SAG AND VISCOSITY CONTROL About twelve years ago a Unton Carbide exploration geologist was tramping through central California In search of nickel or other metallic mineral deposits which would be of value to che Corporation. Although neither of us realized It In 1957, what he found Is what I'm here to talk about this evening: CALIDRIA ASBESTOS The word "asbestos" la a conmerclal term applied to several fibroua silicate minerals which are fire-proof and capable of being processed into flexible fibers. Although there are six different varieties of asbestos, chrysotlle is by far the moat coomon and accounts for some 907. of world production. Canada produces 1% million tons per year, while in the United States small quantities are mined in Vermont, Arizona and California. California accounts for over 50% of U.S. production. There are certain characteristics which are unique to chrysotlle asbeatos, and which make it the most-used variety: 1. A lower index of refraction, 1.51 to 1.55 2. Softest and most flexible fibers 3. Positive or cationic surface charge 4. High tensile strength, up to 800,000 pal Figure 1 compares the physical properties of the six different types of asbestos, and you will note the major disadvantage of chrysotlle is poor resistance to acid. However, in spite of this, it is estimated that chrysotlle asbestos is found in over 3000 applications. 2 The Source of CALIDRIA Asbestos is a unique deposit located in the southern part of the Diablo Mountain range, in Fresno and San Benito Counties (see Figure 2). It is in what Is known as the Hew Idrla mining district, which has long been famous as the oldest producing mercury mine In the United States. All exploration activities ware centered in the nearby town of Coalings, and the deposits became known as Coalings Asbestos. The Coalings deposit is unique for several reasons, not the least being that it Is thought to be the largest single mineral deposit in the world. Rich asbestos ore has been found over an area of 40-50 square miles, and to depths of over 500 feet. Conservative estimates Indicate that over one \ hundred million tons of Chrysotlle asbestos are available. Of course Union Carbide does not control all the claims and is not the only company mining the deposit. But, based on exhaustive drilling programs, we feel that we have the richest deposits and ample ore supply for up to one hundred years of operation. Although mine owners try to keep such information confidential, Canada'8 ora reserves have been estimated at less than 50 million tons. Chrysotlle asbestos occurs only in serpentine, a fine-grained rock composed almost entirely of hydrous magnesium silicate minerals similar to chrysotlle in composition. Figure 3 depicts its crystal structure. The Canadian and moat other deposits of serpentina contain chrysotlle in cross-fiber veins chat are rarely more than half an inch thick. A typical ore contains only 6-10% fiber, of random lengths and tightly bonded together in a parallel configuration, (see Figure 4). The Coalinga deposit bears little resemblance to other serpentine bodies found throughout the world since most of the mass has been highly sheared and pulverized. It consists of soft, friable sheets and clumps of asbestos fibers, and the only other known ore body of this type is the Stragari deposit la Yugoslavia. Ia contrast to the cross-iber arrangement of conventional ores, the Coalings deposit occurs as a swirling mesh of dlsorlanted fibers (see Figure 5). Each fiber or fiber bundle is only in point contact with its neighbor. The "fiber assay" of the ore we process ranges from 50-60% and is all classed as short fiber, similar to a Canadian Grade 7. As mentioned before typical Canadian deposits yield varying fiber lengths, ranging from saveral Inches down to several microns. These are designated by Canadian standards from Grade 3 (spinning fibers) to Grade 7 (shorts and floats). In addition to removing large quantities of rock from asbestos fibers, the fibers must also be classified by length. Conventional Canadian processing methods Include blasting, crushing, grinding, and air clasaifylng. Figure 6 shows the result of processing coalinga ore by the very beat dry methods. Fiber bundles are still very much in evidence and the full potential of the fiber cannot be utilized. He mine the asbestos ore by conventional open pit methods. After scraping off 10 to 20 feet of overburden, ripper-equipped bulldozers and selfpropelled scrapers are used to remove the ore from the deposit. The ore is loaded into bottom-dump trailers through a 3/4-inch screen and hauled to the mill site. Because of the high production rates obtainable with a minimum amount of equipment, the mine is operated only during the summer season. InclesMnt weather and poor road conditions preclude efficient operations during other parts of the year. Now let me sumnarlze the unusual characteristics of the Coalinga deposit: 1. All chrysotile 2. All short-fiber 3. Random-oriented fibers 4. Over 50% fiber content 5. About 207. moisture concent -4- To take advantage of the unique features of the Coallnga deposit. Union Carbide developed a hydraulic beneficiation process to provide the product shown in Figure 7. Conventional mineral processing techniques such as wet screening and grinding, are utilized; but the process is proprietary and I cannot describe it in detail. I can say that it consists primarily of three systems: rock-fiber separation, refining, and special treatment. This provides us with three basic product categories: fiber, colloidal and modified. Lets take a close look at the fiber before we proceed to a discussion of particular grades and their various applications. It is this individual fiber, its purity and liberation, which makes CALIDRIA Asbestos different from any other asbestos product available today. \ You will remember from Figure 3, depicting the crystal structure of chrysotile asbestos, that there is a slight curvature in the configuration. This rep resents the tubular form of the fibers, which consist of about ten concentric layers of bruclte (magnesium hydroxide) and silica. The tubes have an external diameter of 260 and an Internal diameter of 110&. Electron micro graphs, recently made in Japan of the ends of the fibers, have proven the tubular theory. The length of the fibers varies greatly, probably from 100 to 1000 times the diameter; but we feel that the average L/D ratio ia about 200. This means that the average fiber length is about 5 microna; and, from this, we have estimated that there are 10^ fibrils in one gram of CALIDRIA Asbestos. (For mathematic buffs this means that if all the fibers in one gram were placed end to end they would stretch out 300,000 miles). But let's look at some more practical and measurable numbers and physical characteristics. From strictly geometrical considerations, an assemblage of closely packed hollow tubes with the diameters mentioned previously 5 would have a surface area of 105 square maters per gram (35m2/g Internal and 70m^/g external). Based on BET-nitrogen tests, our asbastos products have surface areas of 60 to 80m^/g. This compares to 10 to 30m^/g for average Canadian asbestos, and verifies the electron microscope observations that there is little or no foreign material between the fibers. Also, sinea we use a wet process, the tube Interiors are probably cleaned out to some extent. Some interesting values are shown In Figure 8 and should facilitate a comparison between asbestos and materials with which you are more familiar. To susmarlze, CALIDRIA chrysotlle asbestos fibers have the following important characteristics: 1. High surface area, 60-80^/g 2. High tensile strength, up to 800,000 psl 3. Cationic surface charge 4. Colloidal form, average L/D of 200 5. Extremely high purity, 90-991 fiber 6. Essentially inert 7. High temperature stability to about 700C. 8. Low refractive Index, 1.51-1.55 As I mentioned previously Canadian asbestos is classified by fiber length into Grades 3 through 7, described as follows: Grade 3 - Spinning fibre 4 - Shingle fibre 5 - Paper fibre 6 - Waste 7 - Shorts Grade 7 la divided Into numerous sub-grades, such as: 7D, 7M, 7R, 7T, etc.; which have slightly different characteristics. Figure 9 compares the "average" Canadian Grade 7 with CALIDRIA products. Figure 10 shows all the CALIDRIA products and their major market applications The discussion which follows, to the best of toy ability, will be about products and applications of direct Interest to you. I don't know if the tape joint, or drywall industry is considered to be in the coatings field; if not, it is certainly a related area. Figure 11 shows a typical ready-mix tape joint compound utilizing CALIDRIA S-G 210. The important factor to note is that the S-G 210 content is only one half the usual amount of asbestos used in such a formulation. Mineral content and water demand are maintained constant by Increasing the inexpensive limestone addition. Textured coetings utilize two other products: S-G 130, a coarser grind than S-G 210, and T-13S, a tltanated asbestos product. To digress just a moment, T-135 is colloidal, or High Purity Asbestos co flocculated with anatase TiOj. It was the first of our modified products. Figure 12 is an electron micrograph which shows how the TIO2 particles are dispersed along the fibers. They are bound together by their opposite electrical charge and cannot be separated by mechanical energy. T-135, in the paper Industry, usually replaces TIO2 on a pound-for-pound basis with no loss in brightness or opacity. This is due to the efficient dis persion of the TIO2 by the asbestos fibers. T-135 is just being Introduced to the texture coating formulators and is showing very good promise as a valuable additive. Good body and high brightness can be achieved with a single product. The potential for an asbestos/rutile product is obvious and we are working toward that end. Even though CALIDRIA fiber is very small, the particle size is presently too large for widespread application in finish coatings. 7 especially interior. An application where the particle size has been adequately small to really offer some advantages is in asphalt compounds. CALIDR1A Resin Grade 110 was developed for this application, especially in automobile undercoatings, and has proved to be quite valuable. Figure 13 shows the Improved thicken* lng efficiency of R-G 110 in a coal tar residue (CP-524). Besides offering t good bodying at low concentrations, R-G 110 is essentially non-abrasive and meets the demanding performance of airless spray applications. Viscosity and thixotropy are two very important words used when talking about liquid resin systems. Viscosity, of course, is a measure of a material's resistance to flow; or, as Webster so aptly puts it: "the state of being viscous". (You can check this when you get home, but he defines VISCOUS as "having viscosity".) Webster, at least in his Collegiate Edition, avoids thixotropy completely; but it is a property which is required in a coating, so we can't ignore it. A thixotropic resin is one which is "thin" when energy is applied, such as pumping or spraying; but "thick" under static conditions. You might think of catsup as thixotropic: thick in the bottle, but when you apply energy to the bottom--look out! A better example might be DuPont's Lucite paint, or approved equal, which spreads easily with just the energy from a brush stroke; although, in the can, it looks like paste. Resin-Grade 144 la a particularly effective thixotrope and viscosity control agent for epoxy resin systems. Figure 14 depicts some of its typical physical characteristics. It disperses readily in liquid resins and hardeners with a Cowles Dissolver or similar high-shear mixer, and over-mixing does not destroy its effect. Epoxy systems containing R-G 144 have excellent aging characteristics; and, up to 2 or 3 phr, are amazingly clear. 8 Resin stability is the main reason that R-G 144 has been included as the thixotrope in the California Division of Highways specification for adhesives used in applying lane markers. Formulations for both Standard-Set and Rapid-Set adhesives are shown in Figure 15. At storage temperatures which sometimes reach 115F., adhesive components containing pyrogenic silica were subject to drastic changes in thixotropy and viscosity. The state found that not only did R-G 144 provide a stable resin, but it also did not detract from adhesion or strength properties. Processing advantages, including reduced cost, are also realized. Unlike some other thixotropes, R-G 144 is effective with amine hardeners; and no amine salts are required for viscosity build or thixotropic stability. The thickening effect of different thixotropes is shown in Figures 16 & 17. Figures 18 & 19 depict the thixotropic effect of R-G 144 and two other thixotropes in epoxy and hardener respectively. With epoxy/hardener systems, each loaded with 47. R-G 144, 70 mil thicknesses can be held at room temperature; and up to 40 mil thicknesses can be held, sag-free, at 80C. Figure 20 shows the results of soma of these tests. The value of R-G 144 as a thixotrope is not limited to epoxy resin systems, as It performs equally well in many other organic systems. It Is being used as a thickener for greases, bituminous mastics and sealers, butyl rubber and polysulfide sealants, heat curable vinyl plastisols, casein and phenolic adhesives, etc. In addition to viscosity control and thixotropy, R-G 144 also provides some measure of reinforcement. The first single-crystal whiskers used by man were asbestos fibers. As mentioned earlier, the tensile strength of asbestos fibrils has been 9 measured aC more than 800,000 psl, as strong aa the strongest filaments. But so far, strengths achieved in composites do not go beyond those achieved with glass-mat reinforcements. We have found good whisker rein forcement with R-G 144 in rigid vinyls (with excellent see-through up to 30 phr loading), nylon molding compounds, polysulfones and others. The whisker theory says that above some critical volume loading, dis continuous short fibers reinforce a given matrix as well as a continuous one of the same material. This is true because the many short fibers are in such close proximity that the central load bearing portions can transfer an applied load from one to the other without the fiber ends becoming Involved. The basic requirement for most resin systems is that the 4d ratio be at least 90. The R-G fiber, at 200:1, is well above the minimum; and Figure 21 depicts the superior reinforcement of VYNS (a PVC-PVA copolymer) with R-G 144 compared to two Canadian asbestos products. These data represent the first work done in this area and show the distinct advantages of a high purity, fully-liberated fiber product which contains 99% asbestos rather than the 60% normally contained in competitive asbestos products. Only modest improvements are effected in several of the low cost, high volume resins such as styrenes and polyethylenes. However, very impressive results have been achieved in polymers derived from polar monomers, such as phenoxy, polysulfone and nylon. These data are tabulated in Figure 22. Dramatic increases in tensile, flexural, and impact strength are effected with additions of 15-307. R-G 144. In Nylon-6, R-G 144 imparts improvements very similar to chopped glass, at considerably less cost. Similar improve ments have also been found in Nylon 6/10 and 6/6. Although R-G 144, at high loadings, is effective in thick*;.Ing polyester 10 - resin systems, it was apparent that this product could not compete with existing thixotropes in such applications. Through the efforts of Dr. Steve Chvastiak of our Niagara Falls R & D staff, another "new" asbestos product was developed. R-G 244 is a chemically modified fiber developed to provide maximum thickening efficiency and thixotropy in polyester spray-up and hand lay-up laminating resins. Figure 23 compares the thickening efficiency of R-G 244 and pyrogenic silica in a typical polyester resin. It is also a very effective thickener in vinyl resin sealants and for organosols and plastlsols used in a wide variety of adhesives, coatings, mastics and sealants. Figure 24 depicts a suggested heat-curable vinyl sealant formulation in which R-G 244 imparts a high dagrea of sag control and promotes adhesion. In most systems R-G 244 does not contribute color or opacity. Optimum efficiency, greatest stability, and lowest cost are obtained through the use of sonic dispersars and high energy mixers. However, especially at low viscosity levels, R-G 244 can be incorporated with low shear, propeller-type stirrers. Since R-G 244 Imparts little, if any, color, it is being rapidly accepted as a thixotrope for polyester gel coats. The thixotropic effect which R-G 244 imparts to a polyester resin is depicted in Figure 25. Here you will note that a high shear, where a resin would be sprayed, the viscosity is lover than with pyrogenic silica; and at low shear, where the resin would come to rest on a surface, extremely high viscosity is developed. This prevents sagging and facilitates the maintenance of a smooth uniform coating. You no doubt have noted during my discussion that in almost every application. sag or viscosity control has been an important factor. This physical characteristic is required in almost all liquid systems, aqueous, or resinous; and including coatings, adhesives, sealants, laminates, and molding compounds. And the secret to the success of CALIDRIA Asbestos is related directly to its ultimate purity and fiber liberation. 1 hope that through this paper I have conveyed the idea that CALIDRIA Asbestos fiber is different and that its range of applications is limited only by your imagination. Pig. 1 Pig. 2 Fig. 3 Fig. 4 Fig. 5 Fig. 6 Fig. 7 Fig. 8 Pig. 9 Fig. 10 Fig. 11 Fig. 12 Fig. 13 Fig. 14 Fig. 15 Fig. 16 Fig. 17 Fig. 18 Fig. 19 Fig. 20 Fig. 21 List of Figures Physical Properties of Asbestos Minerals Location of Union Carbide's CALIDRIA Asbestos operation Crystal structure of chrysotile asbestos Electron Micrograph of Canadian Asbestos Ore Electron Micrograph of Coalings Asbestos Ore Electron Micrograph of Dry-processed Coalings Asbestos Ore Electron Micrograph of CALIDRIA Asbestos Fibers Comparative Physical Properties of Well-Known Fibers Physical Properties of Chrysotile Asbestos CALIDRIA Asbestos Market Applications i TJC Ready-Mix Electron Micrograph of Tltanated Asbestos, CALIDRIA Type- T-135 Comparative Thickening Performance of Various Materials In Coal Tar Residue Typical Physical Characteristics - CALIDRIA R-G 144 Epoxy Adhesives for Pavement Markers Effect on Viscosity of Various Thickeners In Bakellte Epoxy Realn ERL-2774 Effect on Viscosity of Various Thickeners In Bakellte Resin Hardener ZZL-0814 Effect on Thixotropy of Various Thlckners In Bakellte Epoxy Resin ERL-2774 Effect on Thixotropy of Various Thlckners In Bakellte Resin Hardener ZZL-0814 Thickening of Blsphenol-Based Resin with R-G 144 & Thickening of Amine Hardeners with R-G 144 Asbestos Reinforce VYNS-Compresston Molded Fig. 22 Fig. 23 Fig. 24 Fig. 25 Mechanical Properties of Injection Molded Samples Comparison of Thickening Efficiency of ResinGrade 244 Asbestos with that of Colloidal Silica in Polyester Resin Typical Heat-Curable Vinyl Sealant Formulation Comparative Thixotropic Characteristics CALIDRIA R-G 244 Vs Pyrogenic Silica \ ss li 1 a sX I X to 0 * *4 <9 9m0 m0 3.8 tuSSMo x*<1 X SI*? 2S2 to to Jto5 X X 4 0 2 o9s "8 a 3a M to 44 1 F le x ib ilit y Very good to o r N to 3 C-J! M N 2* i V% r+> to 404 S 2 a44 6 5 O 0 to 5 S-1 X*4 to>4 X X to 44 Sax * xX mto X 2 4 I O t9o r 0 $ O Xn0 i0to 4kt4o a to to 2 52 x m u i o X a to <44 *4 0 x > X 0 IX Cft 444 0 4fl M 0 OU 44 404 0 2 to u 0 to 0ttoo 9 u 23 a? 0 tXuo tw>o >i to 4 teo too 2^ t9o 0 0 > 3 0 H 3 n > 3* 1 1 f 2 22 0 0 a-a X 0 00 0to 0 to H 2*5 X0 X-XU0 4xj-0J0 Location of Union Carbide's CALIDRIA Asbestos operation Fig. 2 -t UJ o oo > oX > X o cr a x> to o FIGURE 3* C rystal stru ctu re o f chrysottle asbestos. FiS- p " Electron Micrograph of dry processed asbestos fibers Fig. 7 - Electron Micrograph of vet processed Calidria asbestos fibrils 05 CL oo oQ o oo o * o o* * o o On o GO p-> 11 o en o r*. o o o o o CO o u & 3 BVU <s cUBjCNto <4-1 g C3O --o rs O o GOI ovO F Ir o o Cc"* oo oo o oo o o o o u u B *4 sz ue c cno0 U -O 4 u. 3 g 5 zz f* o o 3 0 05 --* B >* z 4J Li 0 o c B >4 a* CHoO CuAO CO < QS a M <; O PHYSICAL PROPERTIES OF CHRYSOTILE ASBESTOS 5XH o o r>*. o UM CO xM 5Ptf CO o1 oi 1 n r*i* sO o auOa3Os* 0* VO n r*. V CuS3J Cd O o vO o CN en CM r* o eg o1 1 CO i m 1 CM CM CO u m CM NO V <0I <n S3 CO < o oes C3 o!N M 2 5CM X A'MS < 3 COO a. i--i H wHZ 8z < 8 t Oa -M3 e b) o38 \ Gs to u* CALIDRIA PRODUCT DESIGNATION S-G 100 S-G 144 S-G 130 S-G 210 HPP HPO T-135-P T-135-0 R-G 110 R-G 144 R-G 244 APPLICATION Vinyl asbestos and asphalt floor tile it i< n ii ii ii Texture coatings, acoustic compounds Tape Joint compounds Pulp and Paper Industry * P & P, waste treatment, pollution control P& P P & P, textured coatings Asphalt compounds, polyester pre-mix Thixotropic thickener, resin systems " " , polyester resins CALIDRIA Asbestos Market Applications Fig. 10 9 STARTING PO INT FORMULATION, 1-GALLON M IX E R , 4 0 0 0 GRAMS DRY WEIGHT <3Sft Aw8J ouo 3a cm o o cn v 3 CrM. C 00 ce m 'JI 3 3V S I |4 3 CO 14 CO 8 X o 9a 9O.X9 X <58 UU 3 00 o cm O AJ CO >> %C3M* o ^X o cm <r oO GO . ^ CO Mo0 o o o CM >> H 8 v uu a. go 3 >s U 3 *33 3 ^4 a 3 s c VM 33 3 U aa A3J *O4 O 33 3 *3 =3 e 3a* 3 -a934a 3 ^o4 <*-s *3 CO O AJ AJ JC 3 00 s *m 33 U3 00 | 1 3b 3 AJ ^34 J3 H 3 <n o pe4 o 3a. CM e 3 co 0 3 o e CO w4 3 b o <o CV O o o o' 3 3- <4- 3O 3 C 300 3U A3J Xpj 5 3 o o CHO o o - CO o o VpOj o o SO CM J]d4 03J 114 3 n3 f3c4 AJ O AJ 3 e 9 uM OO C3 0 O 00 d 3 JS *3 Hd oa. 3 A3J vX3W 3U 3a* A>Js 3 XAJ XAMJ u V9M VMM 3J AJ 3 X3 X w>v H *3 33 uC *0c40 u >3* 33 3X AJ 3 3 /--s 3 3 -ACJ O Eo JS 3 3 p3J U o d 4oH 300 1 uJ AJ 3 mO 3 X 3 b 3 CoM 3 JASJ 1 o >t 9 O vO0 O oO 3 vO o U 3 vO AJ ^4 p4 3 3 oin Q o H CM o o o o om sO p41 3 MO AJ O d 38 O6 O3 <J G O pX4 *3 S 3 M ^4 p4 > C3 <E9 3 8C op4 A*4J u01 3 ow o c CO c <u 3 0) b 00 c H2o 3 ~9 ^O34 M*8+ *4 AJ c *pX4 s e o w 8 pX4 .P-S 8 ^3 P--V JA3CJ AJ AJ U 7 A9J 3 *M3 X 3 AJ 3 U 93 3 a. 0cp0j 8 AJ 3 JASJ y"\ uXpj W 30.^^4 O3J AJ 3 3 JASJ AJ C 3 e3 Xa 3 *3C4 3 -XJ AJ e o z 0 o o 3 p3j o 3 ^4 A3J AoJ mCM <*-N n * O --3 30 334 jSOj vO 1 O3 o am\ A3J AoJ *eo4 c X 3 O> pO 3 J3S AJ p"4 p4 AJ G 3 Xpj JO 3 X vO*O4 AoZ9J moe" cn e u o z 3 41 -o PcVM . u u 9 ^>4 3 O' wV MNM U CO o A9J XX 3 3 8 -O iOJ X z aa w c a <8 CUO V a* CO C0 >01H Ma AJ 9 a U a aX A9J U 9 es as < c3a m cu a 0 01 *">4\ A9J O o sc 4c> 8 cu *3J < 00 cM E M b. **p3J >j -pe34 2p54 J3S 3 U ^34 p-4 p4 VM 01 X 3 3 < *e4 3 *<p34 A U >pa4. ea 82 *p4 3 A3J 3 p4 H p4 3 Xi *G4 B 9 U <pco4 c X k 3 *3 J0S4* ^34 3 <U4 s3 JS a 3 *pU4 53 Xa o u 0a. G 0 3& 6o .e H 3 OC^4M u 1o44 *33 X 3O M a 3 U *C3 3 z J3 3 S 3 44 3M0.<p34 AJ XAJ X00 c 44 3 8X >> X *3 AJ A8J C3 3U 4C4J u *o 30*4G4 3 CM 3 AJ 3 U A9J 3> 3 3X *434 H H 0 3 3 U ^4 9 X A3J o AJ f-2 *3 3 d3 O 0 VO CM I ue 9B u 33 o 3 33 u o o 3 a 8 Cfl CO 3 14AJ z z AJ 4*4 00 8 X3 d u -3 u u 00 3 3 >p4 a k M 3 8 9 3M 3 XX cu B OH 3 AJ J- r4 514 SP> AJ n* *3 U 8 8 p4 3 3 > <44o 3 3 3 > Xk k o C AJ U3 3o cu O O 3 3 9 3 X X Xu* o o VM AJ d U 31 z u 3U o3 AJ o1 3 3d3 43 0 A3J -9a 3 < CO 1 04 C/D s ft* < 3 "-p' * UO4 3 MU X ^84 u AJ d < CJ cs M3 ^4 8 a 3 X *pX4 Hs 3C Cc U 83 9 po4 AJ p4 p34 AMJ o 3 3 'A o 3 3cn CO H 3 3 pc* rs 30 X3 ^4 CM <n cn O X Ov o --* ^4 ^4 03 e z >*s w3 'J '^S* 12 - Electron Micrograph of Titanated. Asbestos, CALIDRIA Type T-135 Viscosity at 2 Rpm., cps. comparative thickening performance Thickener Added, % By Wt. Fig. 13 CALIDRIA R-G 144 Typical Physical Characteristics Specific Gravity Moisture Content, 7. by tft. Surface Area, Sq. meters per gram Reflectance, G.E. Brightness Nature of Surface Charge pH In Water (27. slurry) Bulking Value, gal./100 lb. Oil Absorption (DOP) lb./lOO lb. Refractive Index, n<j 25C. Aspect Ratio (Average L/D) Tensile Strength, psl* Tensile Modulus, psl* Dry Bulk Density, lb./cu. ft. (fully aerated) 2.45 2.0 max. ' 60 approx. 72-76 Electropositive (Cationic) 9.0 4.8 120 1.54-1.56 200:1 824.000 max. (281,000-436,000) 23.2 x 106 4 *1968 Modern Plastics Encyclopedia, p. 594 EPOXY ADHESIVES FOR PAVEMENT MARKERS RAPID SET TYPE: Package A: Epoxy Resla RESIN-GRADE ASBESTOS Titanium Dioxide Package B: Polymercaptan Hardener 2,4,6-Tri(d ime thylaminome thy1)pheno1 Alkyl Subs. Folynnclear Aromatic Oil 2-Ethyl Hexanoic Acid Carbon Black RESIN-GRADE ASBESTOS Glass Spheres STANDARD SET TYPE: Package A: Epoxy Resin Titanium Dioxide RESIN-GRADE ASBESTOS Talc Package B: N-Aminoethyl Piperazine Nonylphenol Carbon Black Talc RESIN-GRADE ASBESTOS Parts by Wt. 100.00 3.00 1.62 60.00 6.00 15.00 0.20 0.05 2.00 36.36 100.00 7.31 5.00 37.64 23.16 52.00 ' 0.22 77.37 1.00 Fig. 15 B R O O K FIE LD VISCO SITY, CPS., at 2 RPM. and 25C. EFFECT ON VISCOSITY OF VARIOUS THICKENERS IN BAKELITE EPOXY RESIN ERL-2774. Fig. 16 B R O O K F IE LD VISCO SITY, CPS., at 2 RPM. and 25C. EFFECT ON VISCOSITY OF VARIOUS THICKENERS IN SAKELITE RESIN HARDENER Z2L-0814 Fig. 17 EFFECT ON THIXOTROPY OF VARIOUS THICKENERS IN BAKELTTE EPOXY RESIN ERL-2774 Q. cc o CN CN * X UJ Q O CoL cc oI- X X H EFFECT ON THIXOTROPY OF VARIOUS THICKENERS IN BAKELITE RESIN HARDENER ZZL-0814 Fig. 19 1 THICKENING OF BISPHENOL-BASED RESINS 1I2*UJ0 I WITH CAUDRIA RESIN-GRADE 144 ASBESTOS Ingredient BAKCUTE ERU2774 CAUDRIA Avoir* Orade 1A4 Asbestos Broekfleld RVP Viscosity, cps. X 10-* 24 hours 7 days 30 days Room Temperature 45 days 100 l RPM. Thixotropic 2 20 CT. 1.) () 34 22 1.5 32 20 1.6 (b) (b) (b) Parts by WaifIn 100 100 23 RPM. 2 | 20 j137 39 132 | 36 Thixotropic 1 RPM. (T. 1.) 2 20 3.5 250 53 3.6 244 54 Thliotrople Indei (T. 1.) 4.7 4.5 (b) | (b) (b) (b) (b) (b) 100 * 4 RPM. 2 20 Thixotropic Index CT. 1.1 464 87 53 430 76 5.7 480 94 5.1 Vertical Dratadown. mil (c) (b) (b) Cb) 125 (b) (b) Cb) 125 Ingredient BAKCUTE ERL.2799 CAUDRtA Raelit. Orade 144 Asbestea Broekfleld RVP VIocoaJty, cpe. X 10-* 24 hours 7 days 30 days Room Tampsrature 45 days 100 RPM. 2 20 18 3.8 16 3.7 (b) (b) Thixotropic Indix a. i.) 4.7 4.3 (b) Parts by Weight 100 100 RPM. 2 Thixotropic RPM. 3 Thixotropic 2 20 38 6.3 CT. r.) 6.0 2 20 70 11 (T.!.) 6.4 35 6.8 5.1 68 12 5.5 (b) Cb) (b) Cb) Cb) Cb) 100 4 RPM. 2 20 Thixotropic Index (T.l.) 91 13 6.9 122 22 5.5 125 25 5.0 Vertical Dratrdewn. mil (c) Cb) (b) Cb) 80 <b) (b) Cb) 70 (a) Thixotropic Index (T. I.) (b) Not run. viscosity at 2 rom. vtecoarty at 20 rpm. (e) Verdes! Drawdown: A 2-inch wide drawdown waa mada on a horizontal aandbiaatad (tool panel. The panel waa im mediately ralaad to a vortical poalbon and any sag noted. If no u| occurred In 10 minutes, the procedure was repeated and tha thickness Increaaed until sagging occurred. ?9f&8& 9 THICKENING of amine hardeners 9 01330 tL with caudria resin-grade 144 asbestos Formuladee Brookfield RVP Vlacesity, cpe. X 10-* 24 hours 7 dsys 30 days Psrta by WL BAKKUTE Z2L-OB14 ...100 CAUDRIA Reein-Qrade 144 Aabaatoa.......................4 RPM. 2 20 Thixotropic Indai (T.l.) 187 36 5.3 172 34 5.1 177 34 5.2 Parts by Win BAKCUTE ZZUOB20.......100 CAUDRIA ReaJivCrade 144 Asbaatoa .................... 4 RPM. 2 20 Thixotropic Index (T.l.) 67 32 2.1 66 32 2.1 67 35 1.9 Parts by WL BAKCUTE ZTL-0BS4.......100 CAUDRIA Reals Orade 144 Aik setae...................... 4 RPM. 2 20 Thixatrapie Index (T.L) 102 23 4.5 104 23 4.6 104 24 4.4 Vertical Drawdown Mil ItIII MlU Room Temperature (R. T.) 50*C. _______________ TM____________ 20 80*C. -- 30 days at R. T. j 70 30 days at 80*C. | -- 40 -- 40 40 40 40 -- 40 40 40 Fig. 20 REINFORCED VYNS-COMPRESSION MOLDED None R-G 144 7RF9 7R05 Tensile Strength,psi. Tensile Modulus, 103 psi. Elongation, X Izod, ft-lb/in. HDT, C. Color Clarity 7600 396 2 0.6 63.0 Lt. Gray Clear 9000 531 3 0.5 69.9 Lt. Tan Clear 7700 470 16 0.5 64.6 Dk. Gray Opaque 7800 490 0.5 63.3 Dk. Gra; Opaque Formulation: VYNS Temex 5 Advastab CH-90 Advastab ABC-18 Stearic Acid Asbestos 100.00 1.20 0.50 0.75 1.00 10.00 Fig. 21 O O O f"4 ON s& o o o ^ O I O irt ^ O H o<n mO -* vO aI o x z OO t oOO OxN O^nHo mo OO ^No O lA CO o co i i n h h a a H>. fOt-h*J* o o OO Or>. N N or*>. o cn i i io h h o oo tel o C3 O i oo m VO CO I CO oc CO *- n o co GO 03 M e|CoM o o S j ConM on i i M Nn* mO 3 Os CO M z a p4 00 a. * CL on F*9^ com 0.0 m X4J 01 0.0 H * X u * OB 00 3 4*14 >1 JJ 0 ^e4 CO c F34 e 4) 3X 41 3 t* 4UJ CO *3 0 x U CO O X F^ A 0 X c o u f4*) p4 CO c 4> H p441 --4 0 C 4> H <4 Li 3 X F4^) Bu 0 3 X p44X b. 4J 00 A1 c o 0o N MM F ig . 22 > VISCOSITY, CPS. X 10"3 (6 RPM.) o 0.5 1.0 1.5 2.0 2.5 3.0 3.5 SOLIDS, PER CENT BYWT. Comparison of Thickening Efficiency of ResinGrade 244 Asbestos with that of Colloidal Silica in Polyester Resin Fig. 23 TYPICAL HEAT-CURABLE VINYL SEALANT FORMULATION Ingredient BAKELITE Vinyl Dispersion Resin QYLF-2 BAKELITE Vinyl Resin Solution VMCC "Elvacite" 2044(a) "Hycar" 1411(b) "Camel White"(c) FLEXOL Plasticizer 10-10 FLEXOL Plasticizer TCP "Monomer X-970"(d) "Mark" LL(e) Resin-Grade 244 Asbestos "Dicup" R() Per Cent by Weight 24.54 3.92 0.98 0.37 29.20 29.20 2.70 4.91 0.49 3.68 0.01 100.00 > .Dissolve BAKELITE Vinyl Resin Solution VMCC in FLEXOL Plasticizer 10-10 at about 100C. Dissolve "Elvacite" 2044 in FLEXOL Plasticizer TCP at 100C. Mix the two solutions and all the other ingredients together in a pony, "Hobart" or similar mixer. (a) Acrylic resin; Du Pont, Wilmington, Delaware (b) Powdered rubber; B. F. Goodrich, Akron, Ohio (c) Calcium carbonate; H. T. Campbell and Son's Corporation, Baltimore, Maryland (d) Polymerizable monomer; Rohm and Haas, Philadelphia, Pennsylvania (e) Stabilizer; Argus Chemical Corporation, Brooklyn, New York (f) Catalyst; Hercules, Wilmington, Delaware Fig. 24 VISCOSITY, CPS. X 1 0 - Comparative Thixotropic Characteristics CALIDRIA R-G 244 Vs Pyrogenic Silica Fig. 25