SU1288184A1 - Method of producing cellulose sulfonates - Google Patents

Abstract

The invention relates to methods for producing cellulose ethers and sulfur-containing acids, which are used as ion exchange materials, drug extenders, antimicrobial agents, as intermediates in the synthesis of cellulose derivatives. The invention makes it possible to reduce the duration of the sulfonation process and to reduce the destruction of cellulose during processing. This is ensured by the fact that cellulose is processed in a mixture of DMF-N O and anhydrId Sulfonic acid in the presence of pyridine and triphenylphosphine in the following ratio of components of the reaction mixture, wt.: Cellulose 1, pyridine 3-9, DMF 7-15, NjO 1 , 7-2,2; Triphenylphosphine 0.2-2.4. Carrying out the process of dry sulphonation in the presence of these reagents makes it possible to obtain cellulose sulfonates with a degree of substitution of 0.2-1.1 at 0–20 ° C for 5–20 min with a decrease in molecular weight by 5–10%. with S Yu QO 00 atL oo 4

Description

This invention relates to the production of cellulose ethers and sulfur containing acids, which are used as ion exchange materials, drug enhancers, antimicrobial agents, and intermediate products in the synthesis of cellulose derivatives.

The purpose of the invention is to reduce the duration of the process and reduce the destruction of the target product. II p and me 1. By May 1. including cellulose pour a mixture of 1.7 mas. , and 7 ma.ch. DMF and mix until dissolved. To the resulting solution is sequentially added 3 mas. pyridine, 0.3 math. while stirring and cooling benzene sulfonic anhydride and 0.2 wt.h. triphenylphosphine. Blend the mixture for 5 minutes at 0 ° C, precipitate the resulting benzene cellulose cellulose with isopropanol, rinse it with isopropanol, and then with ether and dry it under Qum at room temperature. S.Z. 0.3. The molecular weight reduction of cellulose is 5%.

Example p 2. Do the same but example 1 with the difference that the reagents are used in quantity, ma.h N 0. 1,95,, TMF 11, pyridine 6; benzene sulfonic anhydride 1.7; triphenylphosphine 1,3, and the reaction ao mixture is kept for 15 min at C.Z. 0.8 The molecular weight reduction of cellulose is 8%.

PRI me R 3. Proceed analogously to example 1, with the difference that the reagents are used in quantity, wt.ch .: N, 2.2; DMF 15) pyridine 9 benzene sulfonic anhydride 3.1, triphenylphosphine 2.4; and the reaction mixture is held for 25 min at

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VNIIPI USSR State Committee

for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5

Production and printing company, Uzhgorod, st. Project, 4

with

five

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, Ridina, oh

20 S.S.Z. I, 1 Cellulose molecular weight reduction of 10%.

Example 4, Proceed as in Example 3 with the fact that toluene sulfonic anhydride is used as the sulfonating agent. S.Z. 1.05. The molecular weight reduction of cellulose is 9%.

PRI me R 5 Proceed as in Example 3 with the difference that naphthalene sulfone an-, HYDR1SCH is used as the sulfonating agent. S.Z. 0.4. The molecular weight reduction of cellulose is 5%.

Thus, carrying out the sulfonation process under the specified conditions allows reducing its duration to 5–25 min. 50 times in comparison with the known method with an insignificant decrease in the molecular mass of cellulose (by 5-10%).

Claims (1)

Invention Formula A method of producing cellulose sulfonates by treating cellulose with a sulfonating agent in the presence of pi by that.  Ridina, oh differing in order to shorten the process and reduce the destruction of the target product, anhydrous sulfonic acid is used as the sulfonating agent, and the treatment is carried out in a mixture of dimethyl formamide with diazoto tetraoxide and triphenylphosphine in the following ratio of components,% by weight: Cellulose Pyridin3-9 Dimethylformamide 7-15 Tetraoxide of diazot 1,7-2,2- Triphenylphosphine 0,2-2,4