Preparation method of carboxymethyl chitosan

A technology for carboxymethyl chitosan and chitosan, which is applied in the field of preparation of carboxymethyl chitosan, can solve problems such as large consumption, and achieve the effects of low production cost, improved organic solvent and easy operation.

Inactive Publication Date: 2016-10-26
CANGZHOU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the above-mentioned technical problems, the present invention provides a kind of carboxymethyl carboxymethyl alcohol using semi-dry grinding method using chitosan as raw material, which significantly improves the shortcomings of using organic solvents, consuming a large amount of sodium hydroxide and washing ethanol / water in the traditional process. The preparation method of base chitosan

Method used

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  • Preparation method of carboxymethyl chitosan
  • Preparation method of carboxymethyl chitosan
  • Preparation method of carboxymethyl chitosan

Examples

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Embodiment 1

[0013] A preparation method of carboxymethyl chitosan, comprising the steps of: adding sodium hydroxide to chitosan and fully grinding it to make it uniformly mixed, dropping distilled water into it, mixing and grinding it uniformly for 2 hours, placing it for 12 hours for alkalization, and preparing the alkalized chitosan Add monochloroacetic acid to the sugar, grind and mix evenly, the mass ratio of chitosan, sodium hydroxide and monochloroacetic acid is: 1:3.5:3; add distilled water while grinding for 4 hours to obtain carboxymethyl The initial product of chitosan, the initial product of carboxymethyl chitosan was washed with 75% ethanol solution until the supernatant was free of Cl - , filtered by suction, and dried in an oven at 70°C to obtain carboxymethyl chitosan. The carboxylation degree of the obtained carboxymethyl chitosan reaches 1.65, and the viscosity of 1% carboxymethyl chitosan aqueous solution is 83mPa·s.

Embodiment 2

[0015] A preparation method of carboxymethyl chitosan, comprising the steps of: adding sodium hydroxide to chitosan and fully grinding it to make it uniformly mixed, dropping distilled water into it, mixing and grinding it uniformly for 3 hours, standing for 18 hours for alkalization, and preparing the alkalized chitosan Add monochloroacetic acid to the sugar, grind and mix evenly, the mass ratio of chitosan, sodium hydroxide and monochloroacetic acid is: 1:5.5:3; add distilled water while grinding for 6 hours to obtain carboxymethyl The initial product of chitosan, the initial product of carboxymethyl chitosan was washed with 75% ethanol solution until the supernatant was free of Cl - , filtered by suction, and dried in an oven at 60°C to obtain carboxymethyl chitosan. The carboxylation degree of the obtained carboxymethyl chitosan reached 1.68, and the viscosity of 1% carboxymethyl chitosan aqueous solution was 85mPa·s.

Embodiment 3

[0017] A preparation method of carboxymethyl chitosan, comprising the steps of: adding sodium hydroxide to chitosan and fully grinding it to make it evenly mixed, dropping in distilled water, mixing and grinding it evenly for 2.5 hours, placing it for 16 hours for alkalization, and adding to the alkalized shell Add monochloroacetic acid to the polysaccharide, grind and mix evenly, the mass ratio of chitosan, sodium hydroxide and monochloroacetic acid is: 1:4.5:3; grind for 5 hours while adding distilled water to obtain carboxymethyl Base chitosan initial product, wash carboxymethyl chitosan initial product with 75% ethanol solution until the supernatant is free of Cl - , filtered by suction, and dried in an oven at 60°C to obtain carboxymethyl chitosan. The carboxylation degree of the obtained carboxymethyl chitosan reaches 1.73, and the viscosity of 1% carboxymethyl chitosan aqueous solution is 89mPa·s.

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Abstract

The invention relates to a preparation method of carboxymethyl chitosan, and particularly relates to a preparation method of the carboxymethyl chitosan with a semi-dry grinding method. The preparation method includes the steps of: 1) adding sodium hydroxide to chitosan and fully grinding the components to uniformly mix the components, adding distilled water and uniformly mixing and grinding the components for 2-3 h, and allowing the mixture to stand for 12-18 h for alkalization; 2) adding monochloroacetic acid to the alkalized chitosan, uniformly grinding and mixing the components, wherein the molar ratio of the chitosan, the sodium hydroxide to the monochloroacetic acid is 1:3.5-5.5:3; and 3) dropwisely adding distilled water and meanwhile grinding the mixture for 4-6 h to prepare a carboxymethyl chitosan initial product, washing the carboxymethyl chitosan initial product with an organic solution, and performing suction filtration and drying to prepare the carboxymethyl chitosan. The preparation method has simple operations, wherein only is a less amount of water employed as a reaction medium, so that a large use amount of organic solvent is avoided. The method is low in production cost and environment pollution and is high in synthesis efficiency and productivity.

Description

technical field [0001] The invention relates to a preparation method of carboxymethyl chitosan, in particular to a preparation method of carboxymethyl chitosan using a semi-dry grinding method. Background technique [0002] Carboxymethyl chitosan (CMC for short) is an important derivative of chitosan, which has good water solubility, antibacterial, moisture absorption, film-forming, chelating and other properties, making it widely used in daily necessities, chemicals, agriculture, Widely used in food processing, medicine, environmental protection and other fields. [0003] At present, the preparation method of carboxymethyl chitosan is mainly organic solvent method: using chitosan or chitin as raw material respectively, taking ethanol, isopropanol, DMSO and other organic solvents as reaction medium, alkalization with concentrated alkali, adding a Chloroacetic acid makes it react with chitosan or chitin to prepare carboxymethyl chitosan. The main disadvantages of the abov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
CPCC08B37/003
Inventor 刘长霞闫俊琴王焕云
Owner CANGZHOU NORMAL UNIV
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