Document v11ZM48KeqOvp68Kr5RrJ8749

R. D. Alaburda October 1975 Chambers Works 234-049 340/459 200 1-1-1 "LITHOSOL11 RED 4B ACID . (4-Aminotoluene-3-su!fonic Acid Purified) Principle 4-Aminotoluene-3-sulfonic acid crude is dissolved in water as the sodium salt by the addition of soda caustic liquid. Darco and Super Cel are added to absorb the colored impurities and to aid filtration. The solution is heated*to 95C, filtered, and the filtrate acidified with sulfuric acid to precipitate 4-amino-toluene-3-sulfonic acid as the free acid. After cooling, the 4-aminotoluene-3-sulfonic acid is isolated in a nutsch, dried and ground for sale as "Lithosdl" Red 4B Acid, Reaction The only chemical reaction involved is the conversion of the acid to the soluble sodium salt and, after clarification, the reconversion to the free acid by the addition of sulfuric acid. The product structure is: CH3 4-Aminotoludne-3-sulfonic acid ("Lithosol" Red 4B Acid) M.W. 187.2 R, D. Alaburda October 1975 OPERATING INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED) OPERATION: Chambers Works 234-049 340/459 200 III-l Equipment K-2 p-l TS-15 T-l T-2 P-27 TS-18 P-54 P-45 Bill of Materials (100# Basis) N-l GB-3 N-2 ML-1 * Materials and Orchem Product Code Numbers Lb./ Chg. 4-Aminotoluene-3sulfonic acid crude 049 335 Caustic Soda Liquid 30# 887 500 Sulfuric Acid 945 000 Darco S-51 190 000 Super Cel 946200 2,600 535.5 665 100 50 Product 4-Aminotoluene-3sulfonic acid purified 049 340 "Lithosol" Red 4b Acid 459 200 2,424 2,400 Reference: Chambers Works Process, 049 340/459 200 for the manufacture of "Lithosol" Red 4b Acid/4-Amlnotoluene-3-sulfonic Acid Purified, R.D. Gano, dated August 6, 1974. Batch Size and Yield The Bill of Materials iswritten for a standard 2,400-lb. charge in a 2,800-gal. solution kettle. The charge size may be varied proportionately within the working limits of the available equipment. No goal yield has been established. MU-J1SI RZ DUP050467874 N33032.01 R. D. Alaburda October 1975 OPERATING INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED) OPERATION: Chambers Works 234-049 340/459 200 III-2 m. Hazards Sulfuric acid is a highly corrosive, dangerous liquid. It generates heat on dilution with water. The weak acid attacks most metals with the liberation of flammable hydrogen. The acid attacks and destroys skin tissue. Wear rubber gloves and face shield when handling this material as the minimum protection. "Chem Suits'' should be worn where splashes or leaks are possible. If splashed, wash off with copious amounts of water and report to the hospital. ! Soda caustic liquid is extremely corrosive In contact with all body tissue, whether as liquid or vapor, and even in dilute solutions. It is nonflammable, but generates heat when mixed with acids or water. If splashed, wash off with copious amounts of water and report to the hospital. "Llthosol" Red 4b Acid (4-Amlnotoluene-3-sulfonlc acid) is an aromatic amine' compound which may be hazardous. Avoid contactwith this material. Wear respirator for dust exposure. Waste Disposal The sludge from the clarification press is sent to the dump. The final filtrate is a dilute solution containing sodium sulfate and traces of 4-aminotoluene-3-sulfonic acid. This waste Is run to the plant ditch. Cycle Time The cycle time for beginning of charging In K-2 to shoveling off the nutsch is 24 hours. Drying time is 24 hours. Milling time Is 8 hours. # DUP050467875 R. D. Alaburda October 1975 OPERATING INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-5ULFONIC ACID PURIFIED) OPERATION: Chambers Works 234-049 340/459 200 HI-3 DU P050467876 R. D. Alaburda October 1975 OPERATING! INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED) OPERATION: Chambers Works 234-049 340/459 200 III-4 1. Charge K-2 kettle with 60 inches of water. Turn agitation on. Measure dip on straight side of kettle. .2 Add 166 gallons of Caustic soda to K-2 through meter. (535.5 lbs. 1005t). WEAR RUBBER GLOVES AND FACE SHIELD. ' CAUSTIC SODA IS CORROSIVE AND WILL CAUSE SEVERE BURNS ON THE SKIN. WASH ANY FROM HANDS WITH WATER. REPORT TO MEDICAL DEPT. 3. Start heating K-2 to 90-95C and turn on agitator. Charge in about 2400 lbs. of 4-Aminotoluene-3-Sulfonic Acid Crude. Agitation must be on. 200 lbs. of crude is held out to adjust to test. Use gloves, if dusty use respirator. 4. Check alkalinity on Brilliant Yellow papers. Test must be orange, not red color. 5. Adjust K-2 with balance of crude (200 lbs. held out) and with caustic soda as needed. Use 2600 lbs. crude total. Final alkalinity on Brilliant Yellow Paper must be a light orange, not red. Add crude if test is red. Ad caustic if test Is yellow. .6 Add 100 lbs. Darco. Add slowly--sprinkle. Otherwise foam-over may occur. ,7. Add more water to K-2 to bring volume up to 80 inches total. Measure on straight side of K-2. Stop agitator before measuring. .8 Heat to 95C and hold 1/2 hour. 9. Test for color by filtering a sample. The filtrate should not be darker than a light amber color. Add 50 lbs. more Darco and repeat test If too dark. Check supervision If color remains dark after addition. DUP050467877 R. D. Alaburda October 1975 OPERATING INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED) OPERATION: Chambers Works 234-049 340/459 200 III-5 10. Steam press and lines to be sure they are clear and hot. Lines and press must be hot or plugging will develop. 11. Start pump P-54 and circulate solution to F-l press dressed with cotton duck #10 and back to K-2 until all spigots turn clean and clear. < All Darco must be removed; otherwise* quality will be Impaired. 12. Switch lines to run filtrate to T-l & T-2 dividing the charge evenly. Both tubs will hold the charge from K-2. 13. When K-2 is empty, wash press with hot water back to K-2. Fill K-2 cone. 14. Blow press dry to K-2 and dump to cans. Label cans "Darco Sludge from 4-Aminotoluene-3-sulfonic Acid". It is sometimes necessary to rework Darco sludge to avoid yield loss if the press does not wash properly. Supervision will advise if this is necessary. 15. Turn on agitation. Heat T-i & T-2 with coil steam to 90C to 95C. t Be sure agitation is on. 16. Shut steam off tub coils and start slow addition of sulfuric acid to both T-l & T-2. Acid is added until both tubs are definitely acid (blue) on Congo Red paper. The acid addition should take about one hour. (Stream the size of a pencil.) Be sure steam is off coils or tubs tend to boil over. Temperature must be at 90 to 95C during addition. Shut acid off either tub should it become acid before the other. Do not add an unnecessary excess of acid. WEAR RUBBER GLOVES AND FACE SHIELD. M U-23 *2 DUP050467878 R, Da Alaburda October 1975 OPERATING INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-SULPONIC ACID PURIFIED) OPERATION: Chambers Works 234-049 340/459 200 III-6 17. Cool charge to 25-30C and test for complete precipitation. Additional sulfuric acid added to a sample of filtrate should show no precipitate. 18, Drop charge to either N-l or N-2. Both tubs go on 1 nutsch. 19. Rinse out tubs to nutsch. Avoid using a large quantity of water, no more than' 100 gallons. .20 Put 2 spray washes on the cake on the nutsch and suck dry. Spray 2 to 3 minutes per wash (approximately 250 gallons). .21 Transfer to clean cans. Label M-Aminotoluene-S-Sulfonic Acid Purified Wet". .22 Dry in GB-3 at 100 + 5C. One charge will usually be dried at a time. Follow instructions for graining bowl operation. 23 Dump dry product into clean steel can and allow to cool for milling. Use a respirator and gloves. Dump at 0.5# water or less. Dryer is usually d^y in morning after loading on day shift. 24. Grind on ML-1. Pack product at 225 lbs. net. Sample each charge for: % Purity at lab. One sample for file. Follow separate instructions for milling. 25. Label: "Lithosol" Red 4B Acid. 10 to 12 packs per charge. .26 Containers must be wiped clean before shipping. DUP050467879 R. D. Alaburda October 1975 OPERATING INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED) OPERATION: Chambers Works 234-049 340/459 200 III-7 ANALYTICAL REPORT ar ea j c o s t ronp 1351 INTERMEDIATES SAMPLE OF _______________________bid o . D M A CHARGE NO. PRODUCT CODF KFMT RY* DATE: ANALYZE FOR LITHOSOL RED 4B ACID ^ A. M. p. M. 1 J1 TECH. NO. RESULTS LAB ONLY PURITY **' . SCREEN TEST 40 MESH 60 MESH s 1 M U - 2.1 A I a t*+.7: foci vBOs.'cL. No. yS LOT CHAROK / BUILOINfl / AREA DATE TIME ADDM-L. INTO. / EQUI^HCMT / TAKEN BY HAZARDS TOXIC ET CORROSIVE o TLAMMAVLS o NOH. UAN2UASnUoAL o DUP050467880 R. D. Alaburda October 1975 nCQUCSTED UY' MATERIAL LOCATION (HI OG.f ON NAWK).___ OPERATING INSTRUCTIONS WASTE CHEMICAL TRANSPORTATION ORDER__________ ****._Z"w r* & J/a /AT ---------------------- Chambers Works 234-049 340/459 200 III-8 ___________ . ORDER NO. */7Z^ DATE-- / appr o x . q u an t it y POONUS- GALLONS-- V ^____ FOHM-- MOUIo Q] POWOFII [*] CKANUIIU. AH (' [ t'AS IH [pf'sLUH HY J' | OIIHH ( CONTAINER DRUM OPEN 1 It AD CI.OSILD HEAD LGVERPAK H. G. TANK UNHEATCD HEATED N. G. SLUOGE CAR NO. *jT CONIAiNfcNft > ........... ......... .. UEMPSTFR TANK UMHEAlf.D HCATCD DEMPSTER HOPPER OPEN CLOSED 1HUCK TANK TRAILER UNMfcAfKO HEATED UuVttV **" lUNfAINIUk .MACROS ur.9ft:a inv mfMTAHT fOmo;ivi ___ Vl a mma u s CNAf.u'Ut Elvfe- Ex p l o s .v c DUST CAN CAUSE IT FCrnMft PO.Eaw OAK ON CONTACT WITH AClO I EXPCKORC MAY ALSULT IN 111 AUOF.1 \ TO PE DcLIVEREO TO TRUCK OPEN FLAT OPEN 11 AT WITH TAIL GATE LIFT DUMP PICKUP PICKUP Willi TAIL GA 1'L LIFT THACTON (FORK LIFT WllH LP-UOV "~t>* WsTClT TMACTOJI N. . -.NCiNF. UOUIO WASTE INCINERATOR --TO G BURNED OPF.N PIT 1UASH OU'INT.K--TO Ilf. BOHN* O SLUDGE UlSPOfAL AH*-.A- -DUMP A DUHY OI-KH OITCM MYt CNlt llftffY T ANK TAR PIT ^----- Ri c.rrvto uv-- MU--1123 Contains:__^ **** /** e 3 TL//?.;. J*;J Tn. rz? dc m j/O;_________________________________________________ From:___ 3D/fflA Shtolled Bv < HAZARDS: Corrosive \Y Cyanotic Flammable { J Toxic f1 No Unusual .( ) Haw ___________________________ Other Hazard (Describe) v DUP050467881 R. D. Alaburda October 1975 OPERATING INSTRUCTIONS SUBJECT: "LITHOSOL" RED 4B ACID (4-AMINOTOLUENE-3-SULPONIC ACID PURIFIED) OPERATION: Chambers Works 23^4--0^9 340/459 200 III-9 % "These Operating Instructions have been issued after a full review of current technology and building experi ence as of ^(date), and conform with the current process technology as recorded." __(Supervisor's signature) Building Supervisor Senior Supervisor Chief Supervisor Operations Chief Supervisor Tech, or Plant Assist. /lec /paw #4328 Eat Date /a/e/75 Date_ /aik/77 Date itf/Chr MJ~Z9 8 nz DUP050467882