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Preparation method of O-carboxymethyl chitosan resin

A carboxymethyl chitosan and resin technology, which is applied in the field of resin preparation, can solve the problems of O-carboxymethyl chitosan resin adsorption capacity reduction, low mechanical strength, etc., and achieve strong load capacity, good adsorption effect, Good acid and alkali resistance

Inactive Publication Date: 2014-09-17
CHINA PHARM UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the active group (-NH 2 ) is cross-linked, and the adsorption capacity of O-carboxymethyl chitosan resin after cross-linking is generally reduced, and the mechanical strength is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Suspend 10.0g of chitin in 100mL of isopropanol, heat and swell at 55°C for 5h, slowly add 50mL of 60% NaOH solution dropwise, stir well and cool down, then transfer to -20°C refrigerator to freeze overnight, after thawing the next day Slowly add 28.0 g of chloroacetic acid solution dissolved in 20 mL of isopropanol dropwise under ice bath conditions, and then heat and reflux at 60°C for 4 hours after the dropwise addition, pour out the supernatant, and dissolve the precipitate with 60% to 70% ethanol Wash several times, then adjust to neutral with hydrochloric acid, centrifuge to remove the precipitate, precipitate with absolute ethanol, dehydrate with ethanol and acetone, and dry in vacuum at low temperature to obtain O-carboxymethyl chitin.

[0013] Crush the prepared O-carboxymethyl chitin into 50 meshes and suspend in 100mL of isopropanol, slowly add 100mL of 70% NaOH containing protective agent dropwise, heat up to 80°C and heat to reflux for 2 hours, then pour out...

Embodiment 2

[0016] Suspend 10.0g of chitin in 100mL of isopropanol, heat and swell at 55°C for 7 hours, slowly add 50mL of 40% NaOH solution dropwise, stir evenly, cool down, then transfer to -20°C refrigerator to freeze overnight, and thaw the next day Slowly add 28.0g of chloroacetic acid solution dissolved in 20mL of isopropanol dropwise under ice-bath conditions, and then heat and reflux at 50°C for 6h after the dropwise addition, pour out the supernatant, and dissolve the precipitate with 60% to 70% ethanol Wash several times, then adjust to neutral with hydrochloric acid, centrifuge to remove the precipitate, precipitate with absolute ethanol, dehydrate with ethanol and acetone, and dry in vacuum at low temperature to obtain O-carboxymethyl chitin.

[0017] Crush the prepared O-carboxymethyl chitin into 50 mesh and suspend it in 100mL of isopropanol, slowly add 100mL of 50% NaOH containing protective agent dropwise, heat up to 70°C and heat to reflux for 4h, then pour out the superna...

Embodiment 3

[0020] Suspend 10.0g of chitin in 100mL of isopropanol, heat and swell at 55°C for 3 hours, slowly add 50mL of 50% NaOH solution dropwise, stir well, cool down, then transfer to -20°C refrigerator to freeze overnight, and thaw the next day Slowly add 28.0g of chloroacetic acid solution dissolved in 20mL of isopropanol dropwise under ice-bath conditions, heat and reflux at 70°C for 2 hours after the dropwise addition, pour out the supernatant, and dissolve the precipitate with 60% to 70% ethanol Wash several times, then adjust to neutral with hydrochloric acid, centrifuge to remove the precipitate, precipitate with absolute ethanol, dehydrate with ethanol and acetone, and dry in vacuum at low temperature to obtain O-carboxymethyl chitin.

[0021] Crush the prepared O-carboxymethyl chitin into 50 meshes and suspend in 100mL of isopropanol, slowly add 100mL of 60% NaOH containing a protective agent dropwise, heat up to 80°C and reflux for 6h, then pour out the supernatant , wash ...

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PUM

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Abstract

The invention provides a preparation method of O-carboxymethyl chitosan resin. The method comprises the following steps: 1) preparing single O-carboxymethyl chitosan by using chitin as a raw material, performing carboxymethylation under relatively high temperature by using chitin as the raw material, and then preparing single O-carboxymethyl chitosan with relatively good selectivity by removing acetamido on a bit C2; 2) preparing the O-carboxymethyl chitosan resin by adopting an emulsification crosslinking method, firstly protecting -NH2 and -COO<-> together by adopting a complex reaction between CuSO4 and -NH2 and -COO<-> of O-carboxymethyl chitosan and a Schiff base reaction between formaldehyde and -NH2 of O-carboxymethyl chitosan; then enabling part of hydroxyl on O-carboxymethyl chitosan molecules to participate a crosslinking reaction by using glutaric dialdehyde as a crosslinking agent, thus preparing the O-carboxymethyl chitosan resin with a net structure; finally washing off Cu<2+> and formaldehyde by using hydrochloric acid to obtain glutaric dialdehyde crosslinked O-carboxymethyl chitosan resin containing a great number of active groups. The prepared O-carboxymethyl chitosan resin provided by the invention contains amino groups and carboxyl groups, can be connected with various biological active substances, has relatively good adsorption effects on acid radical ions and protein, has strong load capacities on heavy metal ions, can be bio-degraded, is good in acid resistance and alkali resistance, and can be applied to the field of foods, medicines and chemical industries.

Description

technical field [0001] The present invention relates to a kind of preparation method of resin, relate in particular to a kind of Cu 2+ , formaldehyde, glutaraldehyde cross-linked O-carboxymethyl chitosan resin preparation method. Background technique [0002] Carboxymethyl chitosan is a water-soluble chitosan derivative, which has gradually gained popularity in the medical field because of its good water solubility, film-forming properties, moisture retention, biocompatibility, non-toxicity and biodegradability. Pay attention to. Since there are 2 hydroxyl groups in the molecular structure of chitosan (C 3 bit and C 6 position) and 1 amino group (C 2 position), carboxymethylation can occur at all three positions. Therefore, the products are N, O-CMC, N-CMC and O-CMC. O-CMC is a biodegradable positive polysaccharide containing both active amino groups and carboxyl groups. It can be connected with a variety of biologically active substances in medicine, greatly improving...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08J3/00C08L5/08C08B37/08
Inventor 陈昂孙进王莉尹鸿萍侯惠民彭秀兰沈妙根张军姜红玲
Owner CHINA PHARM UNIV
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