Document XzBKM2ZY4pnBMpDgxj559daRJ

FOR DU PONT USE ONLY TEST AUTHORIZATION NO. TA-C- dat e . .ZSr.m.. February 20, 1976 Su OFFICIAL PRODUCT NAME . Quatamine Solution PRODUCT CODE NO. ________ 345 400 _ POUNDS.PRODUCT PROPOSED . AREA "Ponsol" BUILDING NAME Colors TITLE Modified Quatamine manufacture. 1,070 (2 charges) PREPARED BY: C. J. Brown RESPONSIBLE FOR TEST AND TEST CONCLUSION: - T. Brown p u r p o s e o f t e s t : To demonstrate a revised procedure for Quatamine solution for the Chambers Works and Manati; to demonstrate the substitution of Nucjoar SA for Nuchar C-115N in the clarification step. d u r at io n o f t es t : Two charges ' f s t an d ar d in v o l v ed : Chambers Works process 770-873-100 dated 3/12/75; TA-C-74-777 dated 8/21/74. ANALYTICAL CONTROL OR SPECIFICATIONS: [ ] No change &] Change described under Test Details PROCESS HAZARDS REVIEW: [] Required before test &] Not required MATERIAL SAFETY DATA SHEET: [] Revision required S3 No change PACKAGING ANO SHIPPING CLASSIFICATIONS: [] Revision required W No change H t e c h n ic a l b a s is f o r c h a n g e: OCNB 2966. In laboratory studies Nuchar SA gave equiva lent or superior performance to Nuchar C-115N which is no t es t d et ail s : longer available. (Include Safety and Waste Disposal) See attachment. Safety: The clarified Quatamine solution and filter press sludge are acidic with the equivalent of 6 to 7% hydrochloric acid in the solution. Avoid skin contact. Wear goggles and rubber gloves. . Waste Disposal: 300 lbs. of Nuchar SA, 30 lbs. of SLtper-Cel and associated hydrochloric acid and reaction, by-products remain in the press from a double charge of Quatamine solution. They will be drummed off for disposal. DISTRIBUTION: V. G. J. L. R. T. C. H. T. E. Witterholt Files Gilsdorf Lake Lewis J. R. McCloskey D. O. Miller (2) M. S. Moores D. Putnam (3) V. F .-Ringleb R. F. Stalzer . F. Laucius C. J. Brown APPROVED BYad SR. SUPVR.. MANUFACTURING 1' DT V/ CHIEF SUPVR.. MANUFACTURING DA TE /%>AUTHORIZED BY* / %,/. ^ J/*'JtaP*1 SUFT/.-. MANUFACTURING /lu DATE *M4RK "n u t r e q u ir e d *' w h er e a p p l ic a b l e SOPT./clT. SUPVR .. TECH./PLT. ASSIST. DATE NOT REQUIRED. QUAL1TY CONTROL OR ANALYTICAL* DAre NOT REQUIRED, GEN. SUFT. , ma n u f a c t u r in g * dat e NOT REQUIRED. MANUFACTURING ma n a g e r * NOT REQUIRED, TECHNICAL DIVISION* NOT REQUIRED, PLANT MANAGE** DATE DATE DATE N32987 DUP050467677 Page 2 TA-C-76-197 Quatamine Solution Specifications: No specifications exist for this product at present. Proposed specifications are described below. These- are similar to those for Manati process Quatamine described in TA-C-74-777. 1. It shall be an amber to dark brown solution containing no visible insolubles. t 2. It shall contain 4.5 1.5% hydrochloric acid by Orchem Method 25-204-10-1 (potentiometric titration with .sodium hydroxide solution - under development). 3. It shall contain 21.0 1.0% active ingredient on an as is basis as determined by Orchem Method 2-16-2A (sodium nitrite titration). The following are for guidance only pending further analytical work: 1. It shall contain a maximum of 7.0% staining impurity based upon 100% Quatamine concentration by Orchem Method 25-204-98-1 (HPLC method under development). 2. Limits on % residual N-acetyl Quatamine and AA Phenacyl Chloride will be established by Orchem Method 25-179-98-1. Test Detailsi: Process Steps and Limits Quaternization 1. To the quaternization kettle, add 25 lbs. of process water .0 (temperature < 35C.) and 580 lbs. net of dry acetylaminophenacyl chloride (h A Phenacyl Chloride); then seal the kettle and add 1125 lbs., het of 25% trimethylamine solution (3 drums). Before adding the three drums take a sample from each drum and send to G.A.L. for "Percent TMA" (Orchem Method 15-11-15-1). Label the sample "CORROSIVE". Also submit individual samples from two additional drums of 25% trimethylamine for "Percent TMA". Theca TMA analyses are used to determine the total amount of TMA to be added.for the quaternization. The small amount of water is added to fill the bottom outlet to minimize pluggage. DUP050467678 Page 3 TA-C-76-197 Quatamine Solution 1. Continued. The kettle must be closed before trimethylamine addition to prevent fumes from entering the work ing area. Addition of the amine is currently performed by siphoning. 2. Start the agitation and hold the reaction mass at 25-30C. for 3 to 4 hours. After this pefiod, add additional 25% trimethylamine to the slurry so that a total of 380 20 lbs. (100%) of trimethylamine is added in Steps 1 and 2. Normally another 375 lb. drum of 25% trimethylamine is.sufficient. Continue stirring for an additional 10-12 hours, after which sample the charge for ."Completeness of Quaternization" (Orehem Method 6-11-2, which is the spectrophotometric measurement of the residue obtained from drowning the sample in water). 3. Resample the charge after two hours if the "Completeness of Quaternization" is below 95%. Submit the sample for "Com pleteness of Quaternization" and "Percent TMA" (Orchem Methods 6-11-2 and 15-11-15-1). If the "Completeness of Quaternization" is still below 95%, add 200 lbs.- of trimethylamine solution, stir two hours and resample. Hydrolysis 4. When the quaternization is above 95%, add 280 20 lbs. of 31% hydrochloric acid. Agitate for 10 minutes. Measure the pH. The pH should be 3.5 - 5.0. If higher than 5.0, add 31% hydrochloric acid in 42 lb. increments until the pH is in the range of 3.5 to 5.0. Part of the 280 lbs. of hydrochloric acid may be withheld and final pH adjustment made by small additions. 5. When the pH is at 3.5 - 5.0, add 315 20 lbs. of 31% hydro chloric acid, agitate for 10 minutes, and sample to the analytical laboratory for "Percent HCl" (Orchem Method 71-1-15-1; titration v?ith standard base to methyl red endpoint) . The hydrochloric acid content should be 6-9% (w.w.). If lower than 6.0%, adjust by the addition of 31% hydrochloric acid in 42 lb. increments. The initial charge of hydrochloric acid (Step 4) will neutralize residual trimethylamine. The hydrochloric acid acidification must be carefully controlled to DU P050467679 Page 4 TA-C-76-197 Quatamine Solution 5. Continued. give a molar excess of free hydrochloric acid to N-acetyl Quatamine of approximately 10% to insure complete hydrolysis. The vent valve to the scrubber should be open when sampling and remain open until the charge has been transferred to the hold tank. 6- When the acid strength has been adjusted, heat the charge to 80-85C. and hold for 4 to 4-1/2 hours with agitation. Higher temperatures lead to excessive foaming and lower temperatures increase the hydrolysis time. A minimum of four hours holding time is required to complete hydrolysis. 7. Add 150 lbs. of Nuchar SA and cool the charge to ambient temperature. Do not add any water to dilute the charge. Add a small amount of Nuchar SA initially (3-5 lbs.). Wait until any foaming subsides. Add the remaining Nuchar slowly. If foaming resumes, discontinue the Nuchar addition until it has subsided. Clarification of the Quatamine 8. Add 15 lbs. of Super-Cel to the kettle immediately before filtration. Circulate the charge through the clarification press (dressed with No. 10 cotton duck filter cloth) back to the quaternization tub until the filtrate is clear, then divert the clarified solution to the coupling tub (or holding tub) . Examine the filtrate from the spigot of each plate by collecting a sample in a clean glass jar. 9. When the quaternization tub is empty, charge 300 50 lbs. of process water into the tub. Adjust the temperature to 25-35C. with agitation. Circulate the wash from the kettle through the filter and back to the kettle for at least 30 minutes. Then put the wash into the holding tub with the clarified solution. .. 10. Blow the press with air for 15 minutes to remove any residual solution. The sludge in the press should be removed after two charges of solution have been clarified. The sludge should be discharged into steel drums and sent for disposal. The clarified solution and clarification sludge are highly acidic. Wear rubber gloves and face shield. Avoid physical contact. DUP050467680 Page 5 TA-C-76-197 Quatamine Solution 11. Sample the clarified solution to G. A. L. for % purity by nitrite titration. Label the sample "Corrosive". 12. Repeat Steps 1-11 for a second charge. 13. Depending on the anticipated use of the Quatamine, the double charge may be drummed into plastic lined drums (DRL 391 9001) for l'ater use or used immediately in the manufacture of one of the "Sevron" dyes for which it is an intermediate. DUP050467681