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Preparation of N-sulfonic chitin by high performance positioning

A technology of sulfo-shell and chitosan, which is applied in the field of new high-efficiency positioning preparation of N-sulfo-chitosan, can solve the problems of difficulty in controlling the position and content of sulfonation, inability to orientate sulfonate chitosan, and high cost, and achieve The effect of short production cycle, convenient operation and high content

Inactive Publication Date: 2004-02-04
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has a long cycle, high cost, and it is difficult to control its sulfonation position and content, which will degrade the C on chitosan 3 with C 6 Hydroxyl and C 2 The amino groups on the sulfonate can be sulfonated at the same time, and chitosan cannot be sulfonated at the specified position

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Chitosan with 75% deacetylation degree and 25% SO 3 / DMF (sulfur trioxide / N,N-dimethylformamide) implementation.

[0013] Weigh 2 grams of chitosan with a degree of deacetylation of 75%, grind, suspend in 40 milliliters of water, stir well, adjust the pH value of the suspension to 9-10 with 1 mol / liter sodium bicarbonate solution, and then add 20 milliliters of water , and stirred for 0.5 h. 9.8 g of 25% sulfonating agent SO 3 / DMF was dissolved in 20 ml of water, dropped dropwise into the suspension, and reacted at 65°C for 20 hours. After the reaction was completed, the reaction solution was diluted with deionized water, and then centrifuged to precipitate, and the supernatant was poured until the suspension was gelled. shape, and then the colloidal solution was dialyzed to neutrality with deionized water. The pale yellow product was obtained after filtration and drying.

Embodiment 2

[0015] Chitosan with 92% deacetylation degree and 25% SO 3 / DMF (sulfur trioxide / N,N-dimethylformamide) implementation.

[0016] Weigh 2 grams of chitosan with a degree of deacetylation of 92%, grind, suspend in 40 milliliters of water, stir well, adjust the pH value of the suspension to 9-10 with 1 mol / liter sodium bicarbonate solution, and then add 20 milliliters of water , and stirred for 0.5 h. 9.8 g of 25% sulfonating agent SO 3 / DMF was dissolved in 20 ml of water, dropped dropwise into the suspension, and reacted at 65°C for 20 hours. After the reaction was completed, the reaction solution was diluted with deionized water, and then centrifuged to precipitate, and the supernatant was poured until the suspension was gelled. shape, and then the colloidal solution was dialyzed to neutrality with deionized water. The pale yellow product was obtained after filtration and drying.

Embodiment 3

[0018] Chitosan with 92% degree of deacetylation and 50% SO 3 / DMF (sulfur trioxide / N,N-dimethylformamide) implementation.

[0019] Weigh 2 grams of chitosan with a degree of deacetylation of 92%, grind, suspend in 40 milliliters of water, stir well, adjust the pH value of the suspension to 9-10 with 1 mol / liter sodium bicarbonate solution, and then add 20 milliliters of water , stirred for 0.5 h. 4.9 g of 50% sulfonating agent SO 3 / DMF was dissolved in 20 ml of water, dropped dropwise into the suspension, and reacted at 65°C for 20 hours. After the reaction was completed, the reaction solution was diluted with deionized water, and then centrifuged to precipitate, and the supernatant was poured until the suspension was gelled. shape, and then the colloidal solution was dialyzed to neutrality with deionized water. The pale yellow product was obtained after filtration and drying.

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Abstract

An efficient locating process for preparing N-sulfochitosan includes such steps as suspending the chitosan deacetylated by more than 70% in water to become suspension, using sodium bicarbonate to regulate pH value to 9-10%, dripping the aqueous solution of sulfonating agent (SO3 / DMF), and reacting at 65 deg.C for 15-30 hr. Its advantages are simple process and high purity. It can be used to replace the anticoagulant heparin.

Description

Technical field: [0001] The invention relates to a novel high-efficiency positioning method for preparing N-sulfo chitosan. The obtained product has good anticoagulant property and is a cheap substitute for preparing natural heparin. Background technique: [0002] Chitin is a straight-chain polysaccharide in which N-acetyl-D-glucose is linked by β(1→4) glycosidic bonds. It is widely found in the cell walls of crustaceans, arthropods and fungi, and is second only to cellulose on the earth. One of the most abundant organic compounds. Chitosan, the product of deacetylation treatment of chitin, has some unique physical and chemical properties and physiological functions due to the large number of free amino groups with high activity in its molecular structure. It is widely used in medicine, food, cosmetics, agriculture and environmental protection. It has broad application prospects, especially the chitosan biological health care products made of it have many beneficial effects...

Claims

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Application Information

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IPC IPC(8): C08B37/08
Inventor 田丰刘预胡克鳌赵斌元陈刚
Owner SHANGHAI JIAO TONG UNIV
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