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DMC stem grating esterification chitosan and preparing method thereof

A technology of chitosan and grafted ester, which is applied in the field of fine chemicals, can solve the problems of less research on amphoteric chitosan, and achieve excellent flocculation performance, good bactericidal performance, and high grafting efficiency

Inactive Publication Date: 2017-06-13
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, more studies are conducted on the synthesis of amphoteric chitosan with chloroacetic acid and 3-chloro-2-hydroxypropyltrimethylammonium chloride as raw materials, and chitosan derivatives obtained through esterification and modified with DMC are obtained. The amphoteric chitosan research is less

Method used

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  • DMC stem grating esterification chitosan and preparing method thereof
  • DMC stem grating esterification chitosan and preparing method thereof
  • DMC stem grating esterification chitosan and preparing method thereof

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preparation example Construction

[0030] The present invention also provides the preparation method of above-mentioned DMC grafted esterification chitosan, comprises the following steps:

[0031] Step 1, get 15 parts of paraffin, 0.48 parts of span-60, 0.06 parts of tween-80, after mixing them evenly, add 15 parts of an aqueous solution containing 0.5 parts of O-succinic acid chitosan, wherein O-succinic acid The molecular weight of chitosan is 150,000, the degree of substitution is 0.60, and a mixed solution is obtained.

[0032] Step 2, stir and emulsify the mixed solution for 35 minutes at 30°C, then add 0.015-0.088 parts of initiator cerium ammonium nitrate, and then add 1.5-3.5 parts of monomer DMC dropwise at 40-70°C. It is 5s / drop, and after reacting for 5-8h, it is cooled to obtain a reaction emulsion.

[0033] Step 3, add 30 parts of 95% ethanol solution to the reaction emulsion, let it stand for 1 hour, perform suction filtration, and wash the product of suction filtration with ethanol several times...

Embodiment 1

[0037] The concrete method of the DMC grafted esterified chitosan that preparation grafting efficiency is 36% is

[0038] Step 1, get the paraffin of 15ml, the span-60 of 0.48g, the tween-80 of 0.06g, after it is mixed evenly, after stirring for 20min, add 15ml to contain the aqueous solution of 0.5g O-succinate chitosan, wherein O - Chitosan succinate has a molecular weight of 150,000 and a degree of substitution of 0.60 to obtain a mixed solution.

[0039] Step 2: Stir and emulsify the mixed solution for 35 minutes at 30°C, then add 0.015g of initiator cerium ammonium nitrate, and then add 1.5g of monomer DMC dropwise at 40°C, wherein the dropping speed is 5s / drop, and the reaction After 5h, it was cooled to obtain a reaction emulsion.

[0040] Step 3, add 30ml of 95% ethanol solution to the reaction emulsion, let stand for 1h, carry out suction filtration, and use ethanol to wash the product of suction filtration 3 times, then dry the product to obtain DMC grafted esterifi...

Embodiment 2

[0043]The concrete method that prepares the DMC grafted esterified chitosan that grafting efficiency is 43% is

[0044] Step 1, get the paraffin of 15ml, the span-60 of 0.48g, the tween-80 of 0.06g, after it is mixed evenly, after stirring for 20min, add 15ml to contain the aqueous solution of 0.5g O-succinate chitosan, wherein O - Chitosan succinate has a molecular weight of 150,000 and a degree of substitution of 0.60 to obtain a mixed solution.

[0045] Step 2: Stir and emulsify the mixed solution for 35 minutes at 30°C, then add 0.02g of initiator cerium ammonium nitrate, then add 2g of monomer DMC dropwise at 50°C, where the dropping speed is 5s / drop, and react for 6h Afterwards, cooling was carried out to obtain a reaction emulsion.

[0046] Step 3, add 30ml of 95% ethanol solution to the reaction emulsion, let stand for 1h, carry out suction filtration, and use ethanol to wash the product of suction filtration 3 times, then dry the product to obtain DMC grafted esterif...

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Abstract

The invention discloses DMC stem grating esterification chitosan and a preparing method thereof. The method comprises the step of making O-butanedioic acid chitosan and methacryloxyethyltrimethyl ammonium chloride subjected to a free radical polymerization reaction to prepare DMC stem grating esterification chitosan. The chitosan is high in stem-grating efficiency, large in molecular weight, small in distribution range, and good in flocculation and bactericidal performance. The reaction condition is mild, green and free of pollution, the operation is simple and the reaction time is short.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a DMC grafted esterified chitosan; the invention also relates to a preparation method of the DMC grafted esterified chitosan. Background technique [0002] The quaternization modification of chitosan is an important and earlier chitosan modification method. It introduces quaternary ammonium groups on the amino groups of chitosan, or connects a low-molecular quaternary ammonium salt to chitosan. A class of chitosan derivatives obtained on the sugar backbone. Because the water solubility of quaternized chitosan is better than that of chitin and chitosan, it can better exert the effect of chitosan. The modified chitosan quaternary ammonium salt not only has the properties of typical quaternary ammonium salts, such as antibacterial and antibacterial properties, moisture absorption and moisture retention, but also maintains the original good film-forming, flocculation and biocom...

Claims

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Application Information

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IPC IPC(8): C08F251/00C08F220/34C08B37/08
CPCC08F251/00C08B37/003C08F220/34C08F2500/01
Inventor 郭睿郭煜李云鹏马兰王映月宋博土瑞香韩双
Owner SHAANXI UNIV OF SCI & TECH