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A clean production method of chitosan with high degree of deacetylation

A clean production and high deacetylation technology, applied in the field of marine chemical engineering, can solve problems such as heavy odor, low production efficiency, and difficulty in meeting the requirements of chitosan deacetylation degree

Active Publication Date: 2020-10-23
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are three problems in this process: (1) the chitosan obtained by this process generally has a degree of deacetylation of about 85%, which is difficult to meet the requirements of the medical industry for the degree of deacetylation of chitosan
(2) The reaction time is too long and the production efficiency is low
(3) The reaction is generally carried out in an open container, and the smell is heavy, which brings certain environmental pollution and occupational health risks

Method used

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  • A clean production method of chitosan with high degree of deacetylation
  • A clean production method of chitosan with high degree of deacetylation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 500g chitin, add it into 2.5L NaOH solution with a mass fraction of 15%, soak at 40°C for 3h. Then the material was transferred to a 5L vacuum reaction autoclave, the vacuum pressure was -0.078MPa, and the temperature was 70°C for 2 hours. After the reaction was completed, 2.0 L of NaOH solution was recovered by suction filtration. The chitosan was washed with tap water until neutral, and dried at 105° C. for 4 hours to obtain 408 g of chitosan. The lotion is vacuum concentrated to 300mL, and the reclaimed lye and concentrated lye are combined to obtain 2.3L of NaOH lye (concentration 15%). Add 30g of solid NaOH and 200mL of water to obtain 2.5L of NaOH solution with a mass fraction of 15%. Prepare the next batch of chitosan.

[0019] According to GB29941-2013 detection chitosan sample quality index, the results are as follows:

[0020]

[0021]

Embodiment 2

[0023] Weigh 500g of chitin, add it into 2.5L of KOH solution with a mass fraction of 20%, soak at 50°C for 3h. Then the material was transferred to a 5L vacuum reactor, the vacuum pressure was -0.080MPa, and the temperature was 73°C for 2 hours. After the reaction, 2.1 L of KOH solution was recovered by suction filtration. The chitosan was washed with tap water until neutral, and dried at 105° C. for 4 hours to obtain 400 g of chitosan. The lotion was vacuum-concentrated to 300mL, and the reclaimed lye and concentrated lye were combined to obtain 2.4L of KOH lye (concentration 19%). Add 44g of solid KOH and 100mL of water to obtain 2.5L of KOH solution with a mass fraction of 20%. Prepare the next batch of chitosan. After testing, the deacetylation degree of chitosan is 95.6%, and other indicators meet the requirements of GB29941-2013.

Embodiment 3

[0025] Weigh 500g of chitin, add it into 2.5L of KOH solution with a mass fraction of 25%, soak at 50°C for 1h. Then the material was transferred to a 5L vacuum reactor, the vacuum pressure was -0.085MPa, and the temperature was 80°C for 1.5h. After the reaction, 2.1 L of KOH solution was recovered by suction filtration. The chitosan was washed with tap water until neutral, and dried at 105° C. for 4 hours to obtain 397 g of chitosan. The lotion was vacuum-concentrated to 300mL, and the reclaimed lye and concentrated lye were combined to obtain 2.4L of KOH lye (concentration 23%). Add 73g of solid KOH and 100mL of water to obtain 2.5L of KOH solution with a mass fraction of 45%. Prepare the next batch of chitosan. After testing, the deacetylation degree of chitosan is 97.6%, and other indicators meet the requirements of GB29941-2013.

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Abstract

The invention belongs to the technical field of ocean chemical engineering, and relates to a method for efficiently preparing high deacetylation degree chitosan under a condition of relatively low alkaline concentration. The method comprises the following steps: firstly adopting alkali liquor with the mass fraction of 10% to 25% to carry out soaking pretreatment on chitin, then carrying out deacetylation under negative pressure, and carrying out post-treatment to obtain the chitosan. The method for preparing the chitosan with the deacetylation degree of 95% or more than 95% by directly adopting the chitin under a relatively low alkaline liquor concentration is realized, and the reuse of the alkaline liquor is realized. Compared with the prior art, the production efficiency is improved by two to three times, no liquid waste is generated in the process, and the clean production of chitosan is realized.

Description

technical field [0001] The invention relates to a method for efficiently preparing chitosan with a high degree of deacetylation under the condition of relatively low alkali concentration, which realizes the repeated utilization of lye and the clean production of chitosan, and belongs to the technical field of marine chemical engineering. Background technique [0002] Chitosan is a biological polysaccharide formed by connecting glucosamine and N-acetylglucosamine with β-1,4 glycosidic bonds. It is the only positively charged polysaccharide in nature and has biodegradable, antibacterial, flocculation, and film-forming properties. . At present, chitosan is widely used in food, medicine, environmental protection and other fields. In addition, chitosan can be further degraded into chitooligosaccharides, which can induce systemic resistance in crops, improve the yield and quality of agricultural products, and have great application potential in the agricultural field. [0003] C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
CPCC08B37/003
Inventor 司更花马韵升孙建忠虞凤慧刘海玉陈盼盼张健冯文娟刘结磊韩立霞
Owner CHAMBROAD CHEM IND RES INST CO LTD
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