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Novel preparation method for sulfated chitosan

A technology of chitosan and chitosan, which is applied in the field of preparing sulfated chitosan, can solve the problems of difficult control of the operation process, reagents affecting the application, adverse effects of the application, etc., and achieves low production cost, good immune regulation effect, Sulfate content safe effect

Inactive Publication Date: 2010-08-04
YUNNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These reagents will not only pollute the environment, but also have a strong stimulating effect on human skin, mucous membranes, nerves and other systems, and the residues will adversely affect their applications in food, medicine, bionic materials, etc.
(Chitosan Sulfonation Modification and Application Research, 2007, 24, 1007-2853), Journal of Jilin Institute of Chemical Technology, Wang Cuiyan, etc. adopt concentrated sulfuric acid to synthesize sulfated chitosan, but the concentrated sulfuric acid reaction must be carried out at low temperature, otherwise it will be caused by The carbonization of concentrated sulfuric acid makes the product darker in color, and concentrated sulfuric acid is an inorganic strong acid, which will bring great pollution to the environment
Xihua University Jiang Zhenju et al. (Research on chitosan with sulfuric acid-chlorosulfonic acid mixed esterification, chemical research and application, 2005, 17, 1004-1656) used sulfuric acid-chlorosulfonic acid mixed acid to synthesize sulfated chitosan, but in Inorganic and organic strong acids such as sulfuric acid and chlorosulfonic acid are used in the preparation process, these strong acids will make the reaction very violent, the operation process is difficult to control, and the residues will adversely affect its application in food or medicine
[0004] In short, in the current preparation process of sulfated chitosan, toxic organic solvents such as pyridine and DMF are commonly used, and one of the uses of sulfated chitosan is to use it in food, medicine, and bionic materials, so the residual reagents may will affect its application
In addition, the use of strong acid as a catalyst makes the reaction violent, difficult to control, and pollutes the environment

Method used

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  • Novel preparation method for sulfated chitosan

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Experimental program
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Effect test

Embodiment 1

[0021] Dissolve 1g of chitosan in 100mL of distilled water, then add 0.1mol / L bisulfate solution, stir for 30-60min, adjust the pH with sodium hydroxide; freeze-dry the chitosan-bisulfate solution, The sulfation reaction was carried out under the condition of drying and heating at 80°C for 1 day; after the reaction, the chitosan-bisulfate was dissolved in distilled water and dialyzed for 2 days to remove unreacted bisulfate, and finally freeze-dried to obtain the sulfated shell polysaccharides. Gained sulfated chitosan is analyzed through infrared spectroscopy (IR), and at 1111cm -1 A sulfate group (-SO 3 -) stretching vibration peak; by measuring, the sulfate radical content of sulfated chitosan is 20.4%.

Embodiment 2

[0023] Dissolve 1g of chitosan in 100mL of distilled water, then add 0.1mol / L bisulfate solution, stir for 30-60min, adjust the pH with sodium hydroxide; freeze-dry the chitosan-bisulfate solution, The sulfation reaction was carried out under the condition of drying and heating at 100°C for 1 day; after the reaction, the chitosan-bisulfate was dissolved in distilled water and dialyzed for 2 days to remove unreacted bisulfate, and finally freeze-dried to obtain the sulfated shell polysaccharides. Gained sulfated chitosan is analyzed by IR, at 1111cm -1 A sulfate group (-SO 3 -) stretching vibration peak; by measuring, the sulfate radical content of sulfated chitosan is 18.6%.

Embodiment 3

[0025] Dissolve 1g of chitosan in 100mL of distilled water, then add 0.1mol / L bisulfate solution, stir for 30-60min, then adjust the pH with sodium hydroxide; freeze-dry the chitosan-bisulfate solution, The sulfation reaction was carried out under the condition of drying and heating at 100°C for 2 days; after the reaction, the chitosan-bisulfate was dissolved in distilled water and dialyzed for 2 days to remove unreacted bisulfate, and finally freeze-dried to obtain sulfation Chitosan. Gained sulfated chitosan is analyzed by IR, at 1111cm -1 A sulfate group (-SO 3 -) stretching vibration peak; by measuring, the sulfate radical content of sulfated chitosan is 18.5%.

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Abstract

The invention discloses a novel preparation method for sulfated chitosan. The method comprises the following specific steps: dissolving chitosan in 100ml of distilled water, stirring for 30-60min, and regulating the pH value; carrying out freeze drying on the chitosan-bisulfate solution; heating the freeze-dried sulfated chitosan for 1-5 days under the dry condition, and carrying out sulfation reaction; and carrying out dialyzing and freeze drying to obtain the sulfated chitosan. The invention has the advantages that the organic solvent is not utilized during the preparation process; sulfating products are safe and can avoid environment pollution; the process flow is simple, the conditions are controllable, the production cost is low and the industrialized production can be easily realized; the sulfated chitosan in the invention has good activities of anticoagulation, viral resistance, HIV resistance and the like; and in addition, the sulfated chitosan has the immunoregulation function and good antioxidant activity, and has profound significances on developing antiviral medicines and bionic materials and the like.

Description

technical field [0001] The invention relates to a new method for preparing sulfated chitosan without using an organic solvent. Background technique [0002] Polysaccharides are another important biomacromolecular substances besides proteins and nucleic acids in living organisms. They have the functions of enhancing immunity, anti-aging, anti-oxidation, anti-cancer, anti-rheumatism and preventing AIDS. Sulfated polysaccharides are polysaccharides with sulfate groups on the sugar hydroxyl groups, which have biological activities such as anti-virus, anti-tumor, anti-coagulation and immune enhancement. Japanese scholars have studied the sulfated polysaccharides in seaweed and found that they have anti-tumor effects in vivo. The National Cancer Institute of the United States screened marine invertebrates and found that its aqueous extracts showed strong anti-AIDS virus (HIV) activity, and these active components were basically sulfated polysaccharides. In order to improve the b...

Claims

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Application Information

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IPC IPC(8): C08B37/08
Inventor 李灿鹏赵卉赵改红成伟华张媛圆
Owner YUNNAN UNIV
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