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Chitosan preparation method

A technology of chitosan and carapace, applied in the biological field, can solve the problems of fracture, reduce molecular weight and purity, limit the application scope of products, etc., and achieve the effects of high dissolution rate, improved recovery rate and purity, and low output of acid-base wastewater

Active Publication Date: 2016-12-21
贵州康源生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deacetylation rate of chitosan prepared by this method is relatively high, but due to the use of a large amount of concentrated alkali in the preparation of chitosan, the molecular chain of chitosan is broken in a large number, which reduces its molecular weight and purity, and limits the quality of the product. Application range

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Decalcification: After crushing 10g of insect carapaces, place them in 200g of dilute acid with a mass concentration of 10% and soak for 4 hours at 50°C, filter, wash the filter cake with water for 3-5 times and dry to obtain 7.2g of decalcified Product A;

[0027] (2) Deproteinization: put 7.2g decalcification product A, 0.09g trypsin, 0.09g papain, 0.18g alkaline lipase and 144g water in a three-necked flask, control the pH of the reaction solution to 7.5, and stir at 40°C After hydrolysis for 3 hours, filter, wash and dry the filter cake to obtain 4.3 g of deproteinized product B;

[0028] (3) Purification: 4.3g of deproteinized product B, 28g of hexanoic acid, 22g of oxalic acid, 14g of pyridine and 0.43g of NaCl were stirred and dissolved at 60°C for 3 hours, then filtered, and the filtrate was dried under reduced pressure to remove the solvent, and then passed through NaCl was removed by washing with water, and 3.2 g of chitin was obtained by drying. The HPLC...

Embodiment 2

[0032] (1) Decalcification: After crushing 10g of insect carapaces, place them in 250g of dilute acid with a mass concentration of 15% and soak for 6 hours at 30°C, filter, wash the filter cake with water for 3-5 times and dry to obtain 7.8g of decalcified Product A;

[0033] (2) Deproteinization: put 7.8g decalcified product A, 0.12g trypsin, 0.12g papain, 0.24g alkaline lipase and 78g water in a three-necked flask, control the pH of the reaction solution to 8, and stir at 50°C After hydrolysis for 2.5 hours, filter, wash and dry the filter cake to obtain 5.1 g of deproteinized product B;

[0034] (3) Purification: 5.1g deproteinized product B, 40g hexanoic acid, 32g oxalic acid, 20g pyridine and 1g MgSO 4 , stirred and dissolved at 70°C for 2 hours, filtered, and the filtrate was dried under reduced pressure to remove the solvent, and then washed with water to remove MgSO 4 , dried to obtain 3.8g chitin, the HPLC purity was 93.8%, the recovery rate was 35.6%, and the ash c...

Embodiment 3

[0037] (1) Decalcification: After crushing 10g of insect carapaces, put them in 300g of dilute acid with a mass concentration of 20% and soak for 5 hours at 40°C, filter, wash the filter cake with water for 3-5 times and dry to obtain 6.9g of decalcified Product A;

[0038] (2) Deproteinization: put 6.9g decalcification product A, 0.14g trypsin, 0.14g papain, 0.28g alkaline lipase and water in a three-necked flask, control the pH of the reaction solution to 8.5, stir and hydrolyze at 55°C After 2 hours, filter, take the filter cake and wash and dry to obtain 4.6g of deproteinized product B;

[0039](3) Purification: 4.6g deproteinized product B, 40g hexanoic acid, 32g oxalic acid, 20g pyridine and 1.4g Na 2 SO 4 , stirred and dissolved at 80°C for 1 hour, filtered, and the filtrate was dried under reduced pressure to remove the solvent, and then washed with water to remove Na 2 SO 4 , dried to obtain 3.5g of chitin, the HPLC purity was 93.1%, the recovery rate was 32.6%, a...

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Abstract

The invention provides a chitosan preparation method, which comprises: (1) crushing the shell of the insects, placing in dilute acid, carrying out dipping cooking, filtering, taking the filter cake, and carrying out water washing-drying on the filter cake to obtain a decalcified product A; (2) placing the product A, a compound enzyme and water into a reaction container, hydrolyzing for 2-3 h under a weak alkali condition, filtering, taking the filter cake, and carrying out water washing-drying on the filter cake to obtain a protein removing product B; (3) placing the product B in a mixed solvent, adding a neutral salt, carrying out stirring dissolving for 1-3 h, filtering, carrying out pressure reducing drying on the filtrate to remove the solvent, and carrying out water washing-drying to obtain chitin; and (4) placing the chitin and a NaOH aqueous solution under ultraviolet light, irradiating for 2-3 h while carrying out an ultrasonic treatment, carrying out centrifugation, carrying out water washing on the precipitate to achieve a neutral state, and drying to obtain the chitosan. According to the present invention, the preparation method has advantages of simple preparation process, regular equipment, low production of acid and alkali waste water, and meeting of the green environmental protection production requirement, and the obtained chitosan has advantages of high purity, high molecular weight and high deacetylation degree.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a preparation method of chitosan. Background technique [0002] Chitosan, also known as deacetylated chitin, soluble chitin and polyglucosamine, its chemical name is β-(1→4)-2-amino-2-deoxy-D-glucose, after chitin is treated with concentrated alkali The product obtained by removing the acetyl group. [0003] Chitin, also known as chitin, chitin, etc., is an important component (about 10-30%) of the shells of many lower animals, especially arthropods such as shrimps, crabs, and insects, and also exists in lower plants such as fungi and algae In the cell wall of fungi, it is a natural high molecular polymer linked by β(1→4) glycosidic bonds from the basic units of 2-acetylamino-2-deoxy-D-glucose, and is the only cationic animal fiber found so far and the only alkaline polysaccharide. Chitin and its derivatives have many unique functions and characteristics, and have be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
CPCC08B37/003
Inventor 倪协照
Owner 贵州康源生物科技有限公司
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