Method for continuously preparing chitin/chitosan microsphere materials with different deacetylation degrees

A technology of chitosan microspheres and degree of deacetylation, applied in the field of natural polymers and polymer materials, can solve the problems of increased process and energy consumption, unfavorable large-scale preparation, unfavorable industrial application, etc., and achieves low cost and recycling technology. Proven, reliable, uniform size results

Active Publication Date: 2020-08-11
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Separation and purification steps require additional procedures and energy consumption, which is very unfavorable for large-scale production
[0007] In addition, the current methods for preparing chitin microspheres using NaOH / urea aqueous solution (CN 105771823 A, CN104624130 A) all require strict temperature control in an ice-water bath, which is very unfavorable for industrial applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Shrimp shells are soaked in lye to remove protein, soaked in acid solution to remove inorganic salts, and decolorized with hydrogen peroxide solution to obtain purified chitin. The chitin raw material was added to a concentration of 6.0mol kg -1 The deacetylation reaction occurs by heating in an aqueous potassium hydroxide solution at 80°C for 60 minutes to obtain a mixed solution of chitin and alkali with a degree of deacetylation of about 10%. Cool the mixture to room temperature, remove excess potassium hydroxide aqueous solution by filtering and pressing, add water and a certain amount of urea, and adjust the concentration of potassium hydroxide solution to 3.6mol kg -1 The concentration of urea is 0.3mol kg -1 , rapidly stirring and dissolving at a temperature above the freezing point, and obtaining a chitin solution with a concentration of 4wt% after centrifugal defoaming. After mixing the chitin stock solution with 2 times the volume ratio of the oil phase (oli...

Embodiment 2

[0035] Crab shells are soaked in lye to remove protein, soaked in acid solution to remove inorganic salts, and decolorized with hydrogen peroxide solution to obtain purified chitin. The chitin raw material was added to a concentration of 7.0mol kg -1 Deacetylation reaction is carried out by heating in aqueous potassium hydroxide solution at 80°C for 2 hours to obtain a mixed solution of chitin and alkali with a degree of deacetylation of about 20%. Cool the mixture to below 30°C, remove excess potassium hydroxide aqueous solution by filtering and pressing, add water and a certain amount of urea, and adjust the concentration of potassium hydroxide solution to 3.0mol kg -1 The concentration of urea is 0.6mol kg -1 , rapidly stirring and dissolving at a temperature above the freezing point, and obtaining a chitin solution with a concentration of 0.5wt% after centrifugal defoaming. The hydrophobic membrane with a pore size of 4.7 microns is soaked in the lipophilic substance, so...

Embodiment 3

[0037] The squid bones are soaked in lye to remove protein, and soaked in acid to remove inorganic salts to obtain purified chitin. Add the chitin raw material to a concentration of 8.0mol·kg -1 Deacetylation reaction is carried out by heating in aqueous potassium hydroxide solution at 80°C for 1 hour to obtain a mixed solution of chitin and alkali with a degree of deacetylation of about 30%. Cool the mixture to below 30°C, remove excess potassium hydroxide aqueous solution by filtering and pressing, add water and a certain amount of urea, and adjust the concentration of potassium hydroxide solution to 3.3mol kg -1 The concentration of urea is 0.5mol kg -1 , rapidly stirring and dissolving at a temperature above the freezing point, and obtaining a chitin solution with a concentration of 1 wt% after centrifugal defoaming. The hydrophobic membrane with a pore size of 13 microns is soaked in the lipophilic substance, so that the porous membrane is fully wetted to ensure that th...

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Abstract

The invention discloses a method for continuously preparing chitin/chitosan microsphere materials with different deacetylation degrees. The preparation method comprises the following steps: firstly mixing chitin with a potassium hydroxide solution, heating to carry out deacetylation reaction, then adding water into the mixture of chitosan and the potassium hydroxide solution to dilute to a certainconcentration, cooling, adding a stabilizer, and continuously stirring at a temperature above the freezing point to quickly dissolve the chitosan and the potassium hydroxide solution; and preparing an emulsion from an alkaline aqueous solution in which chitin/chitosan is dissolved and an oil phase through a membrane emulsifier, microfluidic equipment and a conventional stirring device, convertingchitin/chitosan emulsion droplets into chitin/chitosan microspheres by using a coagulator, and washing and drying the microspheres to obtain a microsphere finished product. Functional components areintroduced in the microsphere preparation process, and the functional microsphere material is obtained. The prepared microspheres are carbonized to obtain the nitrogen element doped carbon aerogel microspheres. Discontinuity caused by separation and purification steps in the process of preparing chitin/chitosan microsphere materials with different deacetylation degrees is avoided.

Description

technical field [0001] The invention belongs to the field of natural macromolecules and macromolecular materials, relates to chitin / chitosan microspheres with different degrees of deacetylation, in particular to a method for continuously preparing chitin / chitosan microspheres with different degrees of deacetylation. Background technique [0002] The reserves of chitin and chitosan in nature are a class of natural polymers second only to cellulose. Chitosan is the product of deacetylation of chitin. When the N-deacetylation degree of chitin is above 55%, chitin is transformed into chitosan. [0003] Chitin and chitosan microsphere materials are multifunctional polymer materials with a certain size prepared by dissolving, emulsifying, gelling and other processes with chitin and chitosan as the main raw materials. Chitin and chitosan microsphere materials not only have good biocompatibility and biodegradability, can promote wound healing, have hemostatic effect, and are widely...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14C08B37/08
CPCB01J13/14C08B37/003
Inventor 蔡杰钟奕张俐娜
Owner WUHAN UNIV
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