Preparation method of beta-1,4-glucan-6,2,3-sulfate

A sulfate and dextran technology, applied in the field of β-1, can solve problems such as complicated steps, non-compliance, and no mention, and achieve the effect of simple preparation method

Inactive Publication Date: 2009-06-03
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In foreign countries, there is only the report of preparing anticoagulant cellulose sulfate with cellulose acetate as raw material. This method needs to go through multiple decarboxylation processes, the steps are very complicated, and the product with high degree of substitution cannot be obtained, so its anticoagulant effect is relatively low. Low, in addition, the study did not mention the use of this product in the cosmetics industry
[0005] Sulfated cellulose disclosed in the Chinese patent entitled "Sulfated cellulose and its preparation method and application in the preparation of anticoagulant drugs" is a kind of dextran sulfate with similar structure but different molecular weight and degree of substitution. Anticoagulant drugs, which do not meet the requirements for additives for cosmetic use

Method used

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  • Preparation method of beta-1,4-glucan-6,2,3-sulfate
  • Preparation method of beta-1,4-glucan-6,2,3-sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Preparation of cellulose ionic liquid homogeneous system: add microcrystalline cellulose to ionic liquid 1-butyl-3-methylimidazolium chloride ([Bmim]Cl), in 100°C oil bath at 300r / min Stir at a high speed for 12 hours to dissolve it, and obtain a cellulose ionic liquid homogeneous system;

[0035] (2) Sulfation: Add concentrated sulfuric acid to the cellulose ionic liquid homogeneous system obtained in step (1), the amount of concentrated sulfuric acid is 3.0mol / molAGU (anhydroglucose unit in cellulose); at 35°C, the stirring rate is 800r After carrying out the sulfation reaction under the condition of 1 / min for 8 hours, add 4%, the sodium acetate-ethanol solution of w / v, its consumption is 2 times of reactant volume; The product is precipitated out, and the product is filtered, washed to obtain Crude product of esterification;

[0036] (3) Degradation: the crude product of the esterification product is dissolved in NaH with a pH value of 7.5 2 (PO 4 ) 3 -Na 2 ...

Embodiment 2

[0039] (1) Preparation of cellulose ionic liquid homogeneous system: Add ordinary cellulose to ionic liquid 1-allyl-3-methylimidazole chloride ([Amim]Cl), and heat it in an oil bath at 100°C at 300r / min Stir at a high speed for 12 hours to dissolve it, and obtain a cellulose ionic liquid homogeneous system;

[0040] (2) Sulfation: Add chlorosulfonic acid to the cellulose ionic liquid homogeneous system obtained in step (1), and the consumption of chlorosulfonic acid is 4.5mol / molAGU (anhydroglucose unit in cellulose); After carrying out the sulfation reaction under the condition of 1000r / min for 6 hours, add 4%, the sodium acetate-ethanol solution of w / v, its consumption is 4 times of reactant volume; The product is precipitated out, and the product is filtered, Washing obtains the crude product of the esterification product;

[0041] (3) Degradation: the crude product of the esterification product is dissolved in NaH with a pH value of 9.0 2 (PO 4 ) 3 -Na 2 H(PO 4 ) 3 In...

Embodiment 3

[0044] (1) Preparation of cellulose ionic liquid homogeneous system: add commercially available microcrystalline cellulose to ionic liquid 1-butyl-3-methylimidazole chloride ([Bmim]Cl), Stir at a rate of 300r / min for 12 hours to dissolve it, and obtain a homogeneous cellulose ionic liquid system;

[0045] (2) Sulfation: Add sulfur trioxide to the cellulose ionic liquid homogeneous system obtained in step (1), and the amount of sulfur trioxide is 4.0mol / molAGU (anhydroglucose unit in cellulose); Carry out sulfation reaction under the condition of 900r / min after 7 hours, add 4%, w / v sodium acetate-ethanol solution, its dosage is 3 times of reaction volume; The product is precipitated out, and the product is filtered and washed Obtain the crude product of esterification product;

[0046] (3) Degradation: Dissolve the crude product of the esterification product in NaH with a pH value of 8.0 2 (PO 4 ) 3 -Na 2 H(PO 4 ) 3 In the buffer solution, then add endocellulase 1 (EGL) ...

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Abstract

This invention is about preparation and application of beta-1,4- gluglucosan-6,2,3-sulfuric ester. This preparation is as followings: add cellulose into ion liquid, stir to form the homogeneous system of cellulose and ion, then add sulfation agent, stir at 30-35deg C and 800-1000r / min for 6-8hous. Add the alcohol-alkali liquor to precipitate the product, filter, wash to get raw esterification product. Dissolve it in the NaH2 (PO4)3-Na2H (PO4)3 buffer, PH 7.5. Add EGI to degenerate. We finally get beta-1,4- gluglucosan-6,2,3-sulfuric ester after hyperfiltration grading, condensation with depression and vacuum drying. It could be used as cosmetic additives.

Description

technical field [0001] The present invention relates to a preparation method of β-1,4-glucan-6,2,3-sulfate. Background technique [0002] External environmental pollution, ultraviolet radiation, and changes in the microenvironment of the body will cause the fibrin in the facial microcirculation to be higher than normal, block the blood vessels, cause qi stagnation and blood stagnation, and fail to bring normal nutrients to the skin cells, eventually leading to pigmentation and skin damage. Bleak and lacking in nutrition. Promote the blood circulation of skin microvessels, accelerate the metabolism of cells, restore the elasticity of the rigid blood vessel walls, so that nutrients, water, oxygen and other nutrients can fully reach the elastic fibers and collagen fibers. And maintaining the normal function of these fibers can make the cells active, thereby restoring the bright luster and elasticity of the skin. In other words, beautiful skin lies in the healthy state of bloo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/02A61K31/716A61P17/00
Inventor 李琳王兆梅郭祀远郑必胜肖凯军师少飞李艳毕小玲
Owner SOUTH CHINA UNIV OF TECH
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