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Method for preparing water soluble chitosan

A technology for water-soluble chitosan and chitosan, which is applied in the fields of food preparation, sugar derivative preparation, chemical instruments and methods, etc., can solve the problems of long time consumption and complicated solvent, achieve short time consumption, improve immune function, simple effect

Inactive Publication Date: 2004-12-15
孝感学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It has been reported that the preparation methods of water-soluble chitosan with a higher degree of polymerization are as follows: the first method is to freeze chitin and deacetylate it with strong alkali [Sannan et al.Makromol.Chem., 1976,177:3589 -3600; Kurita et al.Makromol.Chem., 1978:3197-3202], but this method takes too long and requires the use of a large amount of acetone and ether; the second method is to mix chitosan in acetic acid-water- Methanol-pyridine uses acetic anhydride for acetylation reaction [Kurita et al.Chem.Lett., 1989:1597-1598], but the solvent is complex; the third method is to use NaBO 3 First degrade, then acetylate with acetic anhydride in a high-concentration (10%) acetic acid solution, but the amount of acetic anhydride is too large, about 8 to 9 times the molar number of amino groups in chitosan [Kubota et al.Carbohydrate Research, 2000,324:268-274.]; the fourth method is to use enzymes to degrade chitosan with an acetylation degree of 10-30%, and use the difference in the ability of the enzyme to recognize and cut different glycosidic bonds, and the acetylamino group in chitosan Inhomogeneous distribution of raw materials to prepare low molecular weight products, but the yield of water-soluble chitosan products with a degree of polymerization above 10 is generally less than 20% [Qin et al. International Journal of Biological Macromolecules, 2002, 31: 111-117.]

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: Get commercially available shrimp shell chitin 55 grams, with 1000 milliliters of 45wt% sodium hydroxide concentrated solution, react 20 hours at 90 ℃ of temperature, filter, after cleaning lye, chitosan product (degree of acetylation 20%) ) is dissolved with 2500 milliliters of 2wt% acetic acid, filters, adds commercially available hydrogen peroxide 10 grams, reacts at 70 ℃, when chitosan average degree of polymerization drops to 500, adds appropriate amount of sodium bisulfite, then solution is cooled to 5 ℃, dropwise add 1000 ml of ethanol solution containing 12.5 g of acetic anhydride, stir slowly for 12 hours, then slowly stir at 20°C for 24 hours, add alkali to adjust the pH of the reaction mixture to 11 under stirring, add ethanol to settle, centrifuge, and use 0.1wt 500 milliliters of % KOH methanol solution was soaked under stirring, centrifuged, washed three times with 100 milliliters of methanol respectively, drained, and vacuum-dried. The acetyl...

Embodiment 2

[0013] Example 2: Get 110 grams of commercially available crab shell chitin, use 2000 milliliters of 40 wt % sodium hydroxide concentrated solution, react at a temperature of 70 ° C for 12 hours, filter, and after washing the lye with the product (32 percent acetylation), add 2800 Milliliter of 2.6% acetic acid dissolves, filters, and filtrate adds enzyme liquid (produced in Wuhan, contains hemicellulase and chitosanase) to react at 50 ℃, when chitosan average degree of polymerization drops to about 10, then solution is cooled to 0 ℃, dropwise add 2500 milliliters of ethanol containing 24.5 grams of acetic anhydride, stir slowly for 24 hours, then slowly stir for 2 hours at 28°C, add KOH under stirring to adjust the pH of the reaction mixture, add ethanol to settle, centrifuge, and use 0.5wt% 1000 milliliters of KOH ethanol solution was soaked under stirring for one hour, centrifuged, washed three times with 100 milliliters of ethanol respectively, the product was dissolved in ...

Embodiment 3

[0014] Example 3: Get 110 grams of commercially available shrimp chitosan (9% acetylation degree), add 2500 milliliters of 2.9wt% acetic acid to dissolve, filter, add 3 grams of R-10 cellulase (produced in Japan) to the filtrate, and react at 48 ° C , when the average degree of polymerization of chitosan dropped to about 20, then the solution was cooled to 0°C, and 2500 milliliters of ethanol containing 25.1 grams of acetic anhydride was added dropwise, slowly stirred for 12 hours, then temperature controlled to 28°C and slowly stirred for 5 hours, Add KOH under stirring to adjust the pH of the reaction mixture to 9, add ethanol to settle, centrifuge, and soak the solid product in 1000 ml of 0.5wt% KOH ethanol solution for 1 hour under stirring, centrifuge, wash three times with 150 ml of ethanol respectively, add water to dissolve the product, and use NMWL 10kDa , 3kDa and 1kDa ultrafiltration membranes to obtain solutions of three components, after vacuum concentration of the...

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PUM

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Abstract

The process of preparing water soluble chitosan includes adding chitosan into 2-8 wt% concentration acetic acid aqua to compound acetic acid solution of chitosan of 2-10 wt% concentration, adding enzyme or oxidant to degrade chitosan to polymerization degree below 1000, cooling the solution to 0-10 deg.c, adding ethanol or methanol solution of acetic anhydride, stirring first at normal temperature for 2-24 hr and then at 20-40 deg.c for another 20-40 deg.c, adding alkali to regulate pH to over 8 under stirring, adding ethanol to deposit, centrifugation to obtain solid product, soaking in alcohol solution of KOH, centrifugation, alcohol washing, and drying to obtain water soluble chitosan of acetyl degree of 45-55%. The present invention has simple preparation process, and the product is used as material for tumor resisting and immunity raising medicine and health product and as additive for cosmetics and food.

Description

technical field [0001] The invention relates to a new method for preparing water-soluble chitosan (non-salt) with an acetylation degree of 45% to 55% and a polymerization degree of less than 1000. The method simplifies the preparation process of the water-soluble chitosan with a higher polymerization degree and reduces costs. Background technique [0002] Chitin is the second largest natural macromolecular polysaccharide after cellulose on the earth, but macromolecular chitin is insoluble in water and most common organic solvents, which limits its application, so chitin must be chemically modified. Chitosan is the deacetylation product of chitin. Generally speaking, when the degree of polymerization of chitosan is greater than 10, the water solubility is not good, but it can be dissolved in aqueous solutions such as acetic acid, formic acid, and hydrochloric acid. As a natural alkaline polysaccharide, chitosan has some unique functions, but its poor water solubility seriou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A23L29/275C07H1/08C08B37/08
Inventor 覃彩芹鲁黎
Owner 孝感学院
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