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Preparation method of 2-hydroxypropyltrimethyl ammonium chloride chitosan

A technology of hydroxypropyltrimethylammonium chloride and chitosan, which is applied in the preparation of chitosan quaternary ammonium salt, the field of preparation of 2-hydroxypropyltrimethylammonium chloride chitosan, can solve the problem of chitosan Difficult to meet the performance of polysan quaternization products, increase the cost of chemical modification, reduce chitosan grafting efficiency and other problems

Active Publication Date: 2009-12-30
浙江澳兴生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the easy hydrolysis of glycidyl trimethyl ammonium chloride (GTMAC) to form 2,3-dihydroxypropyl trimethyl ammonium chloride under neutral or alkaline conditions, it loses the bond with chitosan (CTS) The ability to combine, and glycidyltrimethylammonium chloride (GTMAC) is also easy to polymerize between molecules in alcohol and water to reduce the grafting efficiency of chitosan (CTS), so that chitosan (CTS) The cost of chemical modification increases, and the performance of the obtained chitosan quaternized product is difficult to meet people's requirements

Method used

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  • Preparation method of 2-hydroxypropyltrimethyl ammonium chloride chitosan
  • Preparation method of 2-hydroxypropyltrimethyl ammonium chloride chitosan
  • Preparation method of 2-hydroxypropyltrimethyl ammonium chloride chitosan

Examples

Experimental program
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Effect test

Embodiment 1

[0052] Chitosan was added to a NaOH solution with a mass fraction of 20%, and the reaction was stirred for 15 hours at a temperature of 110° C. and a pressure of 0.2 Mpa. The supernatant was poured off, and washed with deionized water until neutral. A chitosan with a degree of deacetylation of 90% is obtained.

[0053] Dissolve 5g of chitosan with a deacetylation degree of 90% in an acetic acid solution with a mass fraction of 1%, soak in a water bath at a temperature of 60°C for 5 hours to completely dissolve, vacuum filter, filter out insoluble matter, and add deionized water 40ml of diluted filtrate was poured into a three-necked flask, stirred for 30 minutes, then 80ml of isopropanol was added to separate out chitosan, and 20g of 3-chloro-2-hydroxypropyltrimethylammonium chloride was made into a solution and added in three times. Add once every 2 hours, and each titration time is controlled within half an hour for complex reaction. The reaction temperature is 80°C, and th...

Embodiment 2

[0055] Chitosan was added to NaOH solution with a mass fraction of 20%, and the reaction was stirred for 10 hours at a temperature of 120°C and a pressure of 0.4Mpa, and the supernatant liquid was poured off, washed with deionized water until neutral. A chitosan with a degree of deacetylation of 95% is obtained.

[0056] Dissolve 10g of chitosan with a deacetylation degree of 95% in an acetic acid solution with a mass fraction of 1%, soak in a water bath at a temperature of 60°C for 8 hours to completely dissolve, vacuum filter, filter out insoluble matter, and add deionized water 40ml of diluted filtrate was poured into a three-necked flask, stirred for 30 minutes, then 80ml of isopropanol was added to separate out chitosan, and 50g of 3-chloro-2-hydroxypropyltrimethylammonium chloride was made into a solution and added in three times. Add once every 2 hours, and each titration time is controlled within half an hour for complex reaction. The reaction temperature is 80°C, and...

Embodiment 3

[0058] Chitosan was added to a NaOH solution with a mass fraction of 20%, and the reaction was stirred for 6 hours at a temperature of 115°C and a pressure of 0.3Mpa, and the supernatant liquid was poured off, washed with deionized water until neutral. A chitosan with a degree of deacetylation of 95% is obtained.

[0059] Dissolve 12g of chitosan with a deacetylation degree of 95% in an acetic acid solution with a mass fraction of 1%, soak in a water bath at a temperature of 60°C for 10 hours to completely dissolve, vacuum filter, filter out insoluble matter, and add deionized water 40ml of diluted filtrate was poured into a three-necked flask, stirred for 30 minutes, then 80ml of isopropanol was added to separate out chitosan, and 72g of 3-chloro-2-hydroxypropyltrimethylammonium chloride was made into a solution and added in three times. Add once every 2 hours, and each titration time is controlled within half an hour for complex reaction. The reaction temperature is 80°C, a...

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Abstract

The invention provides a preparation method of 2-hydroxypropyltrimethyl ammonium chloride chitosan and belongs to the technical field of novel biomaterials. The preparation method solves problems of high cost, complex steps, low yield and low performance of obtained quaterisation chitosan products which can hardly meet requirements of people in an existing preparation method of chitosan quaternary ammonium salt. The preparation method of 2-hydroxypropyltrimethyl ammonium chloride chitosan comprises the following steps: A. soaking the chitosan; B. heterogeneous reaction; and C. refining. The preparation method of 2-hydroxypropyltrimethyl ammonium chloride chitosan is achieved by less solvent and high-stability raw materials. The 2-hydroxypropyltrimethyl ammonium chloride chitosan prepared by the method has high yield, higher purity and better quality indexes such as moisture retention, hygroscopicity and microbial resistance.

Description

technical field [0001] The invention relates to a preparation method of chitosan quaternary ammonium salt, in particular to a preparation method of 2-hydroxypropyltrimethylammonium chloride chitosan; it belongs to the technical field of new biological materials. Background technique [0002] Chitosan quaternary ammonium salt is an important class of chitosan derivatives, which inherits the advantages of chitosan such as good biocompatibility and degradability, and also has many new properties, such as good water solubility, retention (Absorptive) hygroscopicity, bacteriostasis, flocculation and stronger electrostatic adsorption have been widely used in the fields of biomedicine, textiles, water treatment materials and environmental protection. Its complexes have been reported in a large number of literatures on pharmaceutical excipients such as genes, drug loading, antibacterial wound materials, and anticoagulant materials. There will be major innovative breakthroughs, and i...

Claims

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Application Information

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IPC IPC(8): C08B37/08
Inventor 王松叶詹金明方维林
Owner 浙江澳兴生物科技有限公司
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