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Preparation method for water-soluble low molecular weight chitosan

A low molecular weight, chitosan technology, applied in the field of chitosan, can solve the problem of difficult recovery of catalysts, and achieve the effects of low production cost and mild reaction conditions

Inactive Publication Date: 2008-08-06
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can effectively degrade chitosan to water-soluble chitosan with a viscosity average mass of about 12,000, the catalyst is difficult to achieve effective recovery.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The first step, 0.050g iron phthalocyanine and 2.0g BMImPF 6 The ionic liquid was put into the reactor and stirred and mixed evenly, and then 5.0 g of 6.0% hydrogen peroxide aqueous solution and 0.10 g of chitosan were added successively;

[0017] The second step is to place the reactor treated in the first step in a water bath with a temperature of 20°C for a constant temperature reaction for 10 minutes, let it stand and cool to room temperature, pour out the supernatant, concentrate it by rotary evaporation, and then add a large amount of absolute ethanol Precipitate water-soluble low molecular weight chitosan.

[0018] The third step is to take the catalytic system and reuse it, and it is not obviously found that the catalytic activity of the catalyst is reduced.

Embodiment 2

[0020] The first step, 0.020g cobalt phthalocyanine and 0.020g HMImBF 4 The ionic liquid was put into the reactor and stirred and mixed evenly, and then 5.0 g of 3.0% hydrogen peroxide aqueous solution and 0.10 g of chitosan were added successively;

[0021] The second step is to place the reactor treated in the first step in a water bath with a temperature of 40°C for a constant temperature reaction for 50 minutes, let it cool down to room temperature, pour out the supernatant, and then add a large amount of absolute ethanol after it is concentrated by rotary evaporation Precipitate water-soluble low molecular weight chitosan.

[0022] The third step is to take the catalytic system and reuse it, and it is not obviously found that the catalytic activity of the catalyst is reduced.

Embodiment 3

[0024] The first step, 0.10g copper phthalocyanine and 0.30g BMImPF 6 The ionic liquid was put into the reactor and stirred and mixed evenly, and then 5.0 g of 6.0% hydrogen peroxide aqueous solution and 0.10 g of chitosan were added successively;

[0025] The second step is to place the reactor treated in the first step in a water bath with a temperature of 90°C for a constant temperature reaction for 20 minutes, let it cool down to room temperature, pour out the supernatant, and add a large amount of absolute ethanol after it is concentrated by rotary evaporation Precipitate water-soluble low molecular weight chitosan.

[0026] The third step is to take the catalytic system and reuse it, and it is not obviously found that the catalytic activity of the catalyst is reduced.

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Abstract

The invention relates to a method for preparing soluble low-molecular-weight chitose via catalyzing, oxidizing and degrading chitose, belonging to the technical field of organic chemical synthesis, which comprises using chitose as material, using metal phthalocyanine dissolved in hydrophobic ion liquid as catalyst and using hydrogen dioxide as oxidant to prepare soluble chitose in a reactor. The invention has mild reaction conditions that can completely degrade chitose into soluble chitose in room temperature and low cost that eliminates adjuvants as dilute hydrochloric acid and caustic soda, while the catalyst system can be separated from reaction system and be repeatedly used.

Description

technical field [0001] The invention relates to a method for preparing water-soluble low-molecular-weight chitosan by catalytic oxidation and degradation of chitosan. The method belongs to the technical field of organic chemical synthesis. Background technique [0002] Chitosan, also known as chitosan, chitosamine, hexanoyl chitin, chitosan, is the product of deacetylation of chitin after concentrated alkali treatment, and is the second largest natural product with annual output after cellulose. Polymer is also the only natural alkaline polysaccharide found so far. However, because of its ordered macromolecular structure, chitosan can only be dissolved in a few dilute acids, but not in water and general organic solvents, which limits its application to a large extent. The low-molecular-weight chitosan obtained through degradation, especially the relative molecular mass at 1×10 4 The following chitosan oligosaccharides are not only soluble in water, but...

Claims

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Application Information

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IPC IPC(8): C08B37/08
Inventor 单永奎赵新华朱海燕施沈一
Owner EAST CHINA NORMAL UNIV
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