Preparation method of epoxy chloropropane cross-linked chitosan microspheres

A technology of epichlorohydrin and cross-linked chitosan, which is applied in chemical instruments and methods, medical preparations of non-active ingredients, pharmaceutical formulas, etc., can solve the problem of large consumption of chitosan and poor adsorption of cross-linked chitosan and other problems, to achieve the effect of strong load capacity, good adsorption, and mild reaction conditions

Active Publication Date: 2012-05-09
ZHEJIANG MARINE DEV RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method utilizes the amino groups on chitosan to react with aldehyde groups to form a Schiff base structure to form network crosslinking. The main disadvantage of this method is that the amino groups on chitosan are consumed in large quantities during the reaction, and there Electronic amino group is an important factor for the adsorption performance of chitosan, and the adsorption of cross-linked chitosan prepared by this method is poor

Method used

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  • Preparation method of epoxy chloropropane cross-linked chitosan microspheres
  • Preparation method of epoxy chloropropane cross-linked chitosan microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Dissolve chitosan powder with a deacetylation degree of 95% in hydrochloric acid with a volume concentration of 1%, and fully stir and dissolve at room temperature to obtain a chitosan sol with a mass fraction of 1%;

[0023] (2) Slowly add the chitosan sol prepared in step (1) to liquid paraffin equal in volume to the volume concentration of 1% hydrochloric acid described in step (1) under stirring conditions, and control the stirring speed to 800 rpm / minute, continue to stir for 10 minutes, the chitosan sol is evenly dispersed in the liquid paraffin, and the chitosan microsphere system is obtained;

[0024] (3) Heat the chitosan microsphere system prepared in step (2) to 50°C, add span80 dropwise to the chitosan microsphere system under stirring conditions, so that the volume fraction of (span80) in the system accounts for 0.1 %, continue to stir to emulsify the chitosan microsphere system for 10 minutes, then add dropwise an ethanol solution of 5% epichlorohydr...

Embodiment 2

[0026] (1) Dissolve chitosan powder with a deacetylation degree of 96% in hydrochloric acid with a volume concentration of 2.5%, and fully stir and dissolve at room temperature to obtain a chitosan sol with a mass fraction of 2%;

[0027] (2) Slowly add the chitosan sol prepared in step (1) to liquid paraffin equal in volume to the volume concentration of 2.5% hydrochloric acid described in step (1) under stirring conditions, and control the stirring speed to 1000 rpm / minute, continue stirring for 15 minutes, the chitosan sol is evenly dispersed in the liquid paraffin, and the chitosan microsphere system is obtained;

[0028] (3) Heat the chitosan microsphere system prepared in step (2) to 53°C, add span80 dropwise to the chitosan microsphere system under stirring conditions, so that the volume fraction of (span80) in the system accounts for 0.13 %, continue stirring to emulsify the chitosan microsphere system for 15 minutes, and then add dropwise an ethanol solution of 10% ...

Embodiment 3

[0031] (1) Dissolve chitosan powder with a deacetylation degree of 98% in hydrochloric acid with a volume concentration of 4%, and fully stir and dissolve at room temperature to obtain a chitosan sol with a mass fraction of 4%;

[0032] (2) Slowly add the chitosan sol prepared in step (1) to liquid paraffin equal in volume to the volume concentration of 4% hydrochloric acid described in step (1) under stirring conditions, and control the stirring speed to 1200 rpm / minute, continue to stir for 10 minutes, the chitosan sol is evenly dispersed in the liquid paraffin, and the chitosan microsphere system is obtained;

[0033] (3) Heat the chitosan microsphere system prepared in step (2) to 55°C, add Tween 80 dropwise to the chitosan microsphere system under stirring conditions, so that (Tween 80) in the system The volume fraction accounts for 0.15%. Continue to stir to emulsify the chitosan microsphere system for 20 minutes, then add dropwise an ethanol solution and calcium carbo...

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Abstract

The invention relates to the technical field of fine and deep processing and utilizing of medicines and aquatic products, and aims at providing a preparation method for preparing cross-linked chitosan microspheres with epoxy chloropropane as a cross-linking agent. The preparation method comprises the steps of: firstly preparing chitosan microspheres by an antiphase suspension method, making partial hydroxy on chitosan molecules to participate in cross-linking reaction with epoxy chloropropane as the cross-linking agent, thus converting linear chitosan molecules into reticular high polymer, and preparing cross-linked chitosan microspheres having a porous reticular structure with calcium carbonate as a pore-forming agent. The cross-linked chitosan microspheres prepared by the preparation method provided by the invention can be biodegraded, have good acid and base resistance, better adsorption effect on acid radical ions and proteins, and strong heavy metal ion loading capacity, and can be applied to foodstuff, medicine chemical industry and other fields.

Description

technical field [0001] The invention relates to the technical field of deep processing and utilization of medicine and aquatic products, in particular to a preparation method of epichlorohydrin cross-linked chitosan microspheres. Background technique [0002] Chitosan is the product of deacetylation reaction of chitin, and its scientific name is β-(1, 4)-2-amino-2-deoxy-D-glucose, which exists in large quantities in marine arthropods such as shrimps and crabs and some In the cell membranes of lower animal fungi, insects, and algae. Chitosan is the only alkaline polysaccharide that exists in nature. It is insoluble in water and alkaline solution, but soluble in most dilute acids such as hydrochloric acid, acetic acid, naphthenic acid and benzoic acid. Its molecules contain -OH, - Functional groups such as NH2, pyran ring, and oxygen bridge are easy to chemically modify, have an exchange effect on anions and cations, and have biocompatibility. Natural chitosan is in powder f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/26C08J3/24C08L5/08C08K5/1515B01J20/24B01J20/28B01J20/30C12N11/10A61K47/36
Inventor 廖妙飞郑斌付万冬杨会成钟明杰周宇芳
Owner ZHEJIANG MARINE DEV RES INST
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