Document V3r4XGEO12jNO62eY8BbEJGyK

I EM I CAL CORPORATION 50 WEST 50TM STREET NEW YORK 20, N. Y. September 26, 1956 *yy,' / Shell Development Company 4560 Horton Street Emeryville 8, California Attentions Mr. C. L. Raymond Gentlemen: ETON ADHESIVE II We have been advised by our Resins and Plastics Sales Department that offtakes of this product are expected to increase appreciably, to about 1 M Lb/M, in the near future. We, therefore, believe that the time is opportune to transfer the manufacture of this product to the PDU at Houston, particularly in view of the poor condition of your equipment as outlined in your letter of August 31, 1956. From previous correspondence, we believe that we have sufficient information concerning the manufacture of Adhesive IX, and we have prepared the usual PDU product transmittal forms, your copies of which are attached. We would like you to review these forms and if any corrections or comments are needed your prompt reply, with copy to our Houston Plant, would be appreciated. Attachments cc - Houston Plant - Manager Manufacturing-Development lam 028997 "N ABS-018203 ENCLOSED WITH:..*--t j4, v ,, " T s HE L L CHEMICAL CORPORATION K'i MOL SHELL OtVLIOttEff CO. PCT .1 .1956 date SEPTEMBER 26, 1956 I ti to HOUSTON PLANT - MANAGER (3) from MANAGER - MANUFAC MENT DEPARTMENT - {feSL'bFF] subject INFORMATION FOR PDI EPON ADHESIVE IX ( -Cl f ,f ire- Transmitted herewith is information concerning the manufac ure and evaluation of Epon Adhesive IX. We believe that the information presented is sufficiently complete to permit preparation and evaluation of t'hls pjrbauTT; Should further information be desired, however, do not hesitate to call on us. In the attached material Sheet One describes the manufacturing pro cedure, Sheet Two describes the testing and evaluation procedures, while Sheet Three describes the raw material position. With the exception of dicyandiamide no new raw materials are intro duced into the PDD with this product. The manufacturer's recommendations re garding dicyandiamide should be noted and observed. Sheet Four concerning shipping and warehousing is not presented since this material is covered in the packaging manual. For this previously marketed product the Resins and Plastics Department of the Chemical Sales Division has no comments to offer, hence Sheet Five, concerning marketing, is not presented. We are, however, transmitting herewith far your background and information a copy of Technical Bulletin SC; 55-47 "Experimental Epon Adhesive IX". Sales of Epon Adhesive IX are estimated to be on the order of 1 H LB/M. We would appreciate your advising us when you consider yourself in * position to manufacture this product on a regular basis A Attachment* if6* (&&) fcdjLdtd-- zc '-/7 BBOj/i* A0' oe + Sheet* 1-3 S'- MrV A* V* Fleer </ SbiU Development - Emeryville (2) Muttffcoturlng Operations - Manager Distribution _n Market Development - Manager Union Tech. Serv. Lab. - Director Houston Research Lab. - " Fu*ph*fin* Store* - * Plastics _n rial Hygiene -n LAM 028998 ABS-018204 Product Development Unit Candidate - Epon Adhesive IX Sheet One: Manufacturing Procedure Compiled by Resin Section - Manufacturing Development Department The manufacturing procedure used by Emeryville is described in the attachmentj this was transmitted to us by Shell Developments* letter of June 22, 1956 which dealt mainly with Epon Resin 562. As has been determined by previous transfers of adhesive manufacture, the changes in kneading equip ment may well require further development work and changes in operating procedure. With regard to the blending of the curing agent - dicyandiamide: Emeryville has been using a colloid mill to obtain the 25#w dicy in Epon 828 concentrate. Since Houston does not have a colloid mill you may wish to attempt to use your small kneaders in a manner similar to your present preparation of Titanox dispersions. Alternately an outside firm, such as REH Dispersions Division of Interchemical, might be used. 9/26/56 lam 028999 Product Development Unit Candidate - Epon Adhesive IX Sheet Two: Testing and Evaluation Procedures Compiled by Resin Section - Manufacturing Development Department Epon Adhesive IX will have the same performance and sales specifications as Epon Adhesive VIII. Since the curing agent is embodied in IX the sample panel preparation procedures should be modified in accord ance with information presented in brochure SC: 55-47 "Experimental Epon Adhesive IX" which is attached. 9/26/56 LAM 029000 Product Development Unit Candidate - Epon Adhesive II Sheet Three: Raw Material Position Compiled by Resin Section - Manufacturing Development Department The recipe for Epon Adhesive IX calls for the following raw materials which are the same as used in the manufacture of Epon Adhesive VIII: Epon 828 Vinylite AYAF Allyl Glycidyl Ether Asbestos Floats In addition, dicyandiamide, pulverized grade, a product of American Cyanamid Company, is also used. A sales brochure covering the material is attached. 9/26/56 LAM 029001 AES-018207 -15- EPON ACHESIVE IX Semi-Scale Manufacturing Practice EPON Adhesive IX is essentially the same formulation as Adhesive VIII except that it contains a dispersed solid catalyst, di- . cyandiamide. It is particularly suited for long, open-assembly time applications, since it will not readily cure at 300*F and temperatures of 3^5-350F are normally required. Formulation of EPON Adhesive IX is certified under MIL-A-833I (USAF) and no modification of the amounts of ingredients are permitted. Process Equipment Blending of the adhesives is carried out in a tilting ReadStandard kneader which is equipped with double sigma blades operating at 21 rpm, external heating coils, and a 7*5 bp motor. The unit has a total capacity of I50 gallons and aworking capacity of 70 gallons if loaded to 0.9 times the10-inch blade radius above the blade centerline. This volume permits theprocessing of a full 500-pound drum of EPON resin and allows the kneader blades to break the surface during the entire addition and kneading time. A drum hoist is provided to charge the mixer, which iB located at ground level. Finished material is dis charged into suitable containers by tilting the mixer. In addition to the above-described mixer, two other pieces of equipment are utilized in the operation. The first of these is a 100gallon stainless steel tank equpped with heating coil and air-driven propeller agitator. This tank is used for pre-dissolving solid resins (i.e., polyvinyl acetate) in the liquid EPON. The second piece of auxiliary equipment is a Morehouse Hy-RSpeed mill equipped with replaceable carborundum stones with variable clearance. This mill is required for premixing of pigment or catalyst with the resin. The procedure for typical batch runs as carried out in plant equipment is as follows: Formulation EPON 828 Vinylite AXAF Allyl Glycidyl Ether Asbestos Dicyandiamide 100 parts by weight 6 2 30 8 LAM 029002 ABS-018208 - 16- Vinyl ite AYAF is dissolved in EPON resin by stirring 30 pounds with 380 pounds of EPON 828 for one hour at 160*C (320#F). The solution i3 transferred to the Read mixer and blended for two hours at about 70C (158F) with 150 pounds of asbestos. In a separate vessel 120 pounds of EPON 828 is heated and mixed at 65-70C (149-158F) with 40 pounds of dicyandiamide (Dicy). The mixture is then passed through the Morehouse mill three times using 60-grit carborundum stones with sufficient clearance to keep the temperature below 70*0. The EPON-Dicy concentrate is then added to the EPON-Vinylite-asbestos mixture in the Read mixer and the charge completed by the addition of 10 pounds of allyl glycidyl ether. Blending at 70#C is continued for one hour to give the finished adhesive. No study has been carried out as to the maximum allowable mixing temperature and all runs to date have been made at temperatures not exceeding 70C. Process Materials EPON 828 and allyl glycidyl ether are supplied by Shell Chemical Corporation. Asbestos 7TF is a product of the Johns-Manville Company and is classified under the designation of "shorts" and "floats". Vlnylite AYAF is obtained from Union Carbide and Carbon Corp. The designation AYAF determines the grade and viscosity of this polyvinyl acetate. Dicyandiamide is a micro-pulverized grade supplied by American Cyanamid Company. Titanium Dioxide is marketed under the trade name of Titanox T i-Fure-R and is supplied by E. I. duPont de Nemours and Co., Ltd. Acetamine Orange is also obtained from duPont under the designa tion of GR Cone 175/0* Testing Each batch of finished adhesive is tested for tensile shear strength and viscosity. Test specimens are cleaned, assembled, and cured as outlined in Shell Chemical Corporation Technical Bulletins SC:52-46, SC:55-29, SC:55-50, and SC:55-47. They are then tested according to MIL-A-833I, which requires certain minimum performance standards. LAW 029003 ABS-018209 -17Viscosities are run after constant temperature (77*F) storage for 48 hours, using a Brookfield Synchro-lectric viscometer with No. 7 Spindle. A maximum viscosity specification of 1 million cp measured at 2 rpm has been Imposed upon Adhesive VI. No maximum has been set for Adhesive VIII and IX. LAM 029004 ABS-018210