Preparation method of carboxymethyl chitosan quaternary ammonium salt in water phase by microwave irradiation

A technology of carboxymethyl chitosan and microwave radiation is applied in the field of preparation of carboxymethyl chitosan quaternary ammonium salt, which can solve the problems of difficult to control experimental conditions, long reaction time, cumbersome steps and the like, and achieves simplified preparation process, The effect of saving reaction time and improving product yield

Inactive Publication Date: 2011-12-07
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are relatively few studies on the preparation method of carboxymethyl chitosan quaternary ammonium salt. The only report about the preparation of carboxymethyl chitosan quaternary ammonium salt is to use traditional heating methods with organic solvents such as isopropanol as the dispersion medium. Prepare the finished product of carboxymethyl chitosan, and then use an organic solvent such as isopropanol as a dispersion medium to quaternize carboxymethyl chitosan to prepare a carboxymethyl chitosan quaternary ammonium salt. A total of more than ten Hours, long reaction time, cumbersome steps, difficult to control experimental conditions, and a burden to the environment
The microwave radiation synthesis method has attracted much attention due to its fast, simple and efficient characteristics. However, so far, there has been no report on the preparation of carboxymethyl chitosan quaternary ammonium salt in aqueous phase by microwave radiation method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1: 2 mL of 40 g / ml NaOH solution was added to 1 g of chitosan (the weight average molecular weight was 320,000, and the degree of deacetylation was 90%) and frozen at -15° C. After natural thawing, add 20mL 5g / ml NaOH solution and stir until the chitosan is evenly dispersed. According to chitosan: chloroacetic acid molar ratio is 1: 3 slowly drips chloroacetic acid solution (purity is greater than 97%), puts into the microwave radiation instrument after stirring evenly and carries out microwave radiation reaction for the first time, and its output power is 200W, radiation The time is 50 min and the temperature is 50°C. The carboxymethyl chitosan product is precipitated with acetone, and then the carboxymethyl chitosan product is dissolved in water to adjust the pH value to 14. According to chitosan and 2,3-epoxypropyltrimethylammonium chloride molar ratio is 1: 10, slowly drips 2,3-epoxypropyltrimethylammonium chloride solution (purity greater than 95%) ), sti...

Embodiment 2

[0014] Example 2: Add 2 mL of 50 g / ml NaOH solution to 1 g of chitosan (weight average molecular weight: 280,000, deacetylation degree: 95%) and freeze at -25°C. After natural thawing, add 10mL 20g / ml NaOH solution and stir until the chitosan is evenly dispersed. According to chitosan: chloroacetic acid molar ratio is 1: 5 slowly drips chloroacetic acid solution (purity is greater than 97%), puts into the microwave radiation instrument after stirring evenly and carries out microwave radiation reaction for the first time, and its output power is 600W, radiation The time is 30 minutes and the temperature is 90°C. The carboxymethyl chitosan product is precipitated with acetone, and then the carboxymethyl chitosan product is dissolved in water to adjust the pH value to 8. According to chitosan and 2,3-epoxypropyltrimethylammonium chloride molar ratio is 1: 12, slowly drips 2,3-epoxypropyltrimethylammonium chloride solution (purity greater than 95%) ), stirred evenly and placed i...

Embodiment 3

[0015] Example 3: 3 mL of 50 g / ml NaOH solution was added to 1 g of chitosan (weight average molecular weight: 220,000, deacetylation degree: 80%) and frozen at -18°C. After natural thawing, add 15mL 60g / ml NaOH solution and stir until the chitosan is evenly dispersed. According to chitosan: chloroacetic acid molar ratio is 1: 8 slowly drips chloroacetic acid solution (purity is greater than 97%), puts into the microwave radiation instrument after stirring evenly and carries out microwave radiation reaction for the first time, and its output power is 500W, radiation The time is 5 minutes and the temperature is 70°C. The carboxymethyl chitosan product is precipitated with acetone, and then the carboxymethyl chitosan product is dissolved in water to adjust the pH value to 9. According to chitosan and 2,3-epoxypropyltrimethylammonium chloride molar ratio is 1: 6, slowly drips 2,3-epoxypropyltrimethylammonium chloride solution (purity greater than 95%) ), stirred evenly and plac...

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Abstract

The invention relates to a microwave radiation preparation method of carboxymethyl chitosan quaternary ammonium salt in water phase. The method uses chitosan as a raw material, chloroacetic acid as a carboxymethylation reagent, and 2,3-epoxypropyltrimethylammonium chloride as a quaternization reagent. Secondary microwave radiation, successive substitution reactions, separation and purification, freeze-drying to obtain carboxymethyl chitosan quaternary ammonium salt. The carboxymethyl chitosan quaternary ammonium salt product has a carboxymethyl substitution degree of 30-90%, and a quaternary ammonium group substitution degree of 15-90%. The preparation of shell carboxymethyl polysaccharide quaternary ammonium salt by the method of the present invention has the characteristics of simple process, short reaction time, high product yield, easy control of reaction conditions, no addition of organic solvents and good repeatability, etc., and has broad application prospects. .

Description

technical field [0001] The invention relates to the technical field of preparation of carboxymethyl chitosan quaternary ammonium salt, in particular to a microwave radiation preparation method of carboxymethyl chitosan quaternary ammonium salt in water phase. Background technique [0002] Chitosan is an alkaline polysaccharide that widely exists in nature. Its molecular structure contains active groups such as amino groups and hydroxyl groups. It can be modified by chemical reactions to make it have more ideal chemical, physical properties and physiological functions. , has broad application prospects in the fields of drug sustained release, functional food, biofunctional materials, cosmetics, sewage treatment and biotechnology. [0003] Carboxymethyl chitosan quaternary ammonium salt is a chitosan derivative that simultaneously introduces carboxymethyl and quaternary ammonium groups on chitosan molecules. Compared with chitosan, carboxymethyl chitosan and chitosan quaterna...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
Inventor 王小英刘博孙润仓
Owner SOUTH CHINA UNIV OF TECH
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