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Esterification and crystallizing process for producing glucose halfaldehyde lactone

A technology of glucuronolactone and process method, which is applied in the field of esterification and crystallization process for the preparation of glucuronolactone, which can solve the problems of difficult product separation, long post-treatment cycle, poor reaction selectivity, etc., and achieve simplified crystallization process flow, avoid dissolution loss, and improve the effect of purity

Inactive Publication Date: 2007-10-31
WUHAN CHEM COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main advantage of this method is that the source of raw material starch is wide and the price is low, but this method has disadvantages such as poor reaction selectivity, incomplete esterification, long post-treatment cycle, difficult product separation, high energy consumption, and low product yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 900ml of oxidized starch hydrolyzate (equivalent to 100g of raw starch) and concentrate the hydrolyzate under reduced pressure at a temperature of 60°C and a vacuum degree of ≥0.09MPa until no visible water distills out. For 48Be. Add 100ml of butyl acetate to the primary concentrate, azeotropically dehydrate at 60°C and a vacuum of 0.08MPa until no liquid distills out, and recover 99ml of butyl acetate. Add 100ml of glacial acetic acid to the secondary concentrate, stir the esterification reaction at 70°C for 1 hour, and then evaporate 20ml of light acetic acid under reduced pressure. The reaction mixture starts to cool down at a rate of 1°C / hour from 70°C and crystallizes under low-speed stirring , when the temperature was 30° C., the crystallization mixture was suction-filtered, the solid was washed with 2×10 ml of absolute ethanol, and dried in vacuo to obtain 20.4 grams of white crystalline powder with a glucuronolactone content of 92%.

Embodiment 2

[0022] Take 900ml of oxidized starch hydrolyzate (equivalent to 100g of raw starch) and concentrate the hydrolyzate under reduced pressure at a temperature of 60°C and a vacuum degree of ≥0.09MPa until no visible water distills out. It is 45Be. Add 120ml of butyl acetate to the primary concentrate, azeotropically dehydrate at 60°C and 0.08MPa vacuum until no liquid distills out, and recover 118ml of butyl acetate. Add 100ml of glacial acetic acid to the secondary concentrate, stir the esterification reaction at 70°C for 1 hour, and then evaporate 20ml of light acetic acid under reduced pressure. The reaction mixture starts from 70°C at a cooling rate of 1°C / hour and stirs at a low speed to cool down and crystallize. When the temperature was 30° C., the crystallization mixture was suction-filtered, the solid was washed with 2×10 ml of absolute ethanol, and dried in vacuo to obtain 23.4 g of white crystalline powder with a glucuronolactone content of 90%.

Embodiment 3

[0024] Take 450ml of oxidized starch hydrolyzate (equivalent to 50g of raw starch) at a temperature of 55°C and a vacuum of 0.093MPa to concentrate the hydrolyzate under reduced pressure until no visible water distills out. For 48Be. Add 50ml of ethyl acetate to the primary concentrate, azeotropically dehydrate at 55°C and 0.07MPa vacuum until no liquid distills out, and recover 45ml of ethyl acetate. Add 50ml of glacial acetic acid to the residue (secondary concentrate), stir the esterification reaction at 68°C for 1.5 hours, and then evaporate 10ml of light acetic acid under reduced pressure. The temperature was lowered to crystallize, and the crystallization mixture was suction-filtered when the temperature was 20° C., the solid was washed with 2×10 ml of absolute ethanol, and dried in vacuo to obtain 9.6 grams of white crystalline powder with a glucuronolactone content of 93%.

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Abstract

Esterifying and crystallizing process for preparing glucuronolactone is carried out by oxidizing by starch acid, hydrolyzing, one-stage concentration dewatering for oxidized starch hydrolysate, two-stage dewatering for one-stage concentrate, adding two-stage concentrate into acetic acid to esterify at 65~70 degrees C, distilling to remove weak acid, third-stage dewatering, lowering temperature, crystallizing by dynamic gradient at 25+-5 degrees C, 1~2 degrees C / hr speed ratio and <=40hrs, filtering to obtain crude product. It is cheap, has less consumption, shorter crystallizing time and more output.

Description

technical field [0001] The invention relates to an esterification process for producing glucuronolactone by an acid method, and a crystallization and purification method for glucuronolactone obtained by the esterification process. The process is a further improvement of the existing process for preparing glucuronolactone esterification and crystallization. Background technique [0002] Glucuronolactone, referred to as glucuronolactone, the molecular formula is C 6 h 8 o 6 , and its chemical composition is: D(+)-glucofuranurono-6,3-lactone]. As a liver detoxifier and immune function regulator, glucuronolactone is a conventional liver-protecting medicine; glucuronolactone and its follow-up products are also the main additives of functional beverages, foods, weight-loss drugs, cosmetics, etc., with The market demand for supplementing physical energy, improving hypoxia, nourishing skin, and delaying aging has exceeded the demand in the medical field in recent years. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/00C07H13/06
Inventor 袁华吴元欣陈启明吴广文闫志国杨小俊孙炎彬
Owner WUHAN CHEM COLLEGE
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