By Peter Simunovich, John-Paul Brisigotti, Mike Haught
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Phosphoric a c i d (85%) gave a very v i s c o u s 2% cellulose s o l u t i o n of practical DP, but the presence of g e l s and fibers made filtration very difficult and H PO could not be washed from f i l m s c a s t on g l a s s p l a t e s . N e u t r a l i z a t i o n w i t h 14% ammonium hydroxide, f o l l o w e d by washing, gave complete removal o f phosphate, but higher concentrations o f ammonium hydroxide gave crystalline ammonium phosphate in the film. 3 4 Table I C r i t i q u e o f C e l l u l o s e Solvents F i r s t Examined Solvent 72% H Result Excessive DP l o s s S 0 2 4 85% H P 0 High g e l and f i b e r , H^PO^ hard t o remove so 2 -NH Good s o l u t i o n , i m p r a c t i c a l to regenerate so 2 - ( C H ) NH Good s o l u t i o n , i m p r a c t i c a l to regenerate 3 4 3 3 2 Good s o l u t i o n , very slow c o a g u l a t i o n 64% ZnCl The extreme difficulty of filtration along with the poor economics a n t i c i p a t e d in u s i n g a 2% solution prompted an exami n a t i o n o f the newer SO -amine s o l v e n t s reported by Hata and Yokota in Japan (1-3).
6. 7. 8. 9. 10. Hata, K. , Sen-i G a k k a i s k i , (1966) 22 ( 2 ) , 96-102. Hata, K. , Sen-i G a k k a i s k i , (1968) 24 ( 9 ) , 415-419. Hata, K. , Sen-i G a k k a i s k i , (1968) 24 ( 9 ) , 420-424. F. S. 2,737,437 dated March 6, 1956. F. S. 2,737,459 dated March 6, 1956. F. S. 2,810,162 dated October 22, 1957. , TAPPI Pasteka, M. and M i s l o v i c o v , , (1974) 8, 107-114. D. , J . A p p l . , A p p l . Polymer Symposia, (1976) 28, 931-943. , J . A p p l . , A p p l . Polymer Symposia, (1976) 28, 945-952.
Unpublished R e s u l t s . ; ACS Symposium Series; American Chemical Society: Washington, DC, 1977. 5 Chemistry of the Cellulose-N2O4-DMF Solution: Recovery and Recycle of Raw Materials NORMAN A. PORTNOY and DAVID P. 07981 The purpose of th tablish a foundation f o r a technically viable recovery and recycle system based on spinning rayon fibers from the cellulose/ N O /DMF s o l u t i o n . Other papers in this symposium d i s c u s s e d solution makeup, s p i n n i n g , and fiber p r o p e r t i e s .