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One-pot homogeneous preparation of chitin and chitosan derivatives with different degrees of deacetylation from chitin

A technology of chitosan derivatives and degree of deacetylation, applied in the field of polymers, can solve problems such as low degree of deacetylation, and achieve the effects of controllable reaction and easy operation

Active Publication Date: 2021-05-04
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method provides a process for the homogeneous preparation of chitin derivatives, but this method can only be used to obtain chitin derivatives with a low degree of deacetylation (≤15%)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add chitin raw material (degree of deacetylation is about 3%) into 40wt% KOH solution and heat at 40°C for 2 minutes to obtain a mixed solution of chitin and alkali with a degree of deacetylation of 5%, cool down to below 30°C, and add a certain amount of The water and urea make the mass fraction of KOH in the solution be 10-25wt%, and the mass fraction of urea be 0-10wt%, stir and dissolve rapidly at a temperature above the freezing point, and obtain a chitin solution with a concentration of 1.0wt% after centrifugal defoaming . According to the material ratio of sodium chloroacetate and chitin monomer unit is 0.5:1, add to the chitin solution obtained above, stir at 0°C for 20h, adjust the pH value of the solution to about 7, purify by dialysis and freeze-dry Carboxymethyl chitin was obtained with a degree of substitution of 0.18.

Embodiment 2

[0027] Add chitin raw material (degree of deacetylation is about 3%) into 40wt% KOH solution and heat at 80°C for 1 hour to obtain a mixed solution of chitin and alkali with a degree of deacetylation of about 10%, cool down to below 30°C, add certain A large amount of water and urea make the mass fraction of KOH in the solution be 10-25wt%, and the mass fraction of urea be 0-10wt%, stir and dissolve quickly at a temperature above freezing point, and obtain chitin with a concentration of 0.5wt% after centrifugal defoaming solution. According to the material ratio of sodium chloroacetate and chitin monomer unit is 0.1:1, add to the chitin solution obtained above, stir at -15°C for 24 hours, adjust the pH value of the solution to about 7, dialysis purification and freezing Dried to obtain carboxymethyl chitin with a degree of substitution of 0.08.

Embodiment 3

[0029] Chitin raw material (deacetylation degree is about 3%) is added to 60wt% KOH solution and heated at 80°C for 30min to obtain a mixed solution of chitosan and alkali with a deacetylation degree of about 60%, cooled to below 30°C, and added A certain amount of water and urea make the mass fraction of KOH in the solution 10-25wt%, and the mass fraction of urea 0-10wt%, stir and dissolve quickly at a temperature above the freezing point, and obtain chitin with a concentration of 1wt% after centrifugal defoaming solution. According to the substance ratio of sodium chloroacetate and chitin monomer unit is 40:1, add to the chitin solution obtained above, stir at 0°C for 24 hours, adjust the pH value of the solution to about 7, purify by dialysis and freeze-dry Carboxymethyl chitosan was obtained with a degree of substitution of 2.12.

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Abstract

The invention discloses a method for homogeneously preparing chitin and chitosan derivatives with different degrees of deacetylation from chitin in one pot. Chitin / chitosan prepared by adding chitin raw materials into a KOH solution with a mass fraction of more than 40% to prepare chitin / chitosan with different degrees of deacetylation is not separated and purified, and is continuously dissolved in a solvent composition containing KOH, a stabilizer and water. The chitin / chitosan solution is obtained, then centrifuged to defoam, and a derivatization reagent is added to obtain chitin or chitosan derivatives. According to the preparation method of the present invention, chitin and chitosan derivatives can be prepared directly using chitin as a raw material in a one-pot method. The operation is simple, the reaction is controllable, energy saving and environmental protection, and multifunctional Chitin and chitosan derivatives.

Description

technical field [0001] The invention relates to a method for homogeneously preparing chitin and chitosan derivatives with different degrees of deacetylation directly from chitin in one pot, and belongs to the field of macromolecules. Background technique [0002] Chitin is a natural polymer material second only to cellulose in nature. It has many special properties, such as biodegradability, biocompatibility and biological activity. important raw material. With the continuous development of new solvents for chitin, new materials such as chitin hydrogels, aerogels, membranes, fibers and microspheres have been widely developed, researched and applied, but it is far from being possible to directly use chitin materials obtained through dissolution and regeneration. far from meeting actual needs. In order to obtain chitin materials with more special functions and properties, molecular design and directional modification of chitin are usually required to meet various specific ne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
CPCC08B37/003
Inventor 蔡杰许唤谢芳张俐娜
Owner WUHAN UNIV