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Cocrystallization technology of glucosamine hydrochloride and glucosamine potassium/sodium sulfate

A technology of glucosamine hydrochloride and glucosamine, which is applied in the direction of amino sugar, crystal growth, sugar derivatives, etc., and can solve problems such as high cost, complicated process, and incomplete reaction of potassium/sodium salt

Inactive Publication Date: 2012-07-18
技源生物制品(徐州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional co-crystallization process is complex, high cost, and potassium / sodium salts cannot fully react, etc.

Method used

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  • Cocrystallization technology of glucosamine hydrochloride and glucosamine potassium/sodium sulfate
  • Cocrystallization technology of glucosamine hydrochloride and glucosamine potassium/sodium sulfate
  • Cocrystallization technology of glucosamine hydrochloride and glucosamine potassium/sodium sulfate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 431.2g (2mol) glucosamine hydrochloride, add 142.0g (1mol) anhydrous sodium sulfate, add 2000ml pure water, heat to 60~65℃, keep the temperature within this range and stir for 1h; then cool to 30~ Filter with a 0.22μm polypropylene filter membrane at 35°C; at 50~70°C, concentrate under reduced pressure until a large amount of crystals appear, stop heating and concentrate, add 1000ml of 95% ethanol, let stand for 12h, centrifuge, and dry the crystals to give 562.7g. The rate is 98.2%.

[0022] The obtained glucosamine sodium sulfate has a content of 99.6%, an optical rotation of +53.1°, a pH of 4.4, an ash content of 24.2%, and a moisture content of 0.2%.

Embodiment 2

[0024] Weigh 431.2g (2mol) glucosamine hydrochloride, add 170.8g (0.98mol) potassium sulfate, add 2000ml pure water, heat to 60~65℃, keep the temperature within this range and stir for 1h; then cool to 30~35 ℃, 0.22μm polypropylene filter membrane; at 50~70℃, concentrate under reduced pressure until a large amount of crystals appear, stop heating and concentrate, add 1000ml of 95% ethanol, let stand for 12h, centrifuge and dry the crystals, get 591.0g, yield It is 97.6%.

[0025] The obtained glucosamine sulfate potassium salt content is 99.3%, the optical rotation is +51.3°, the pH is 4.3, the ash content is 28.5%, and the moisture content is 0.2%.

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Abstract

The invention relates to a cocrystallization technology of glucosamine hydrochloride and glucosamine potassium / sodium sulfate, which is characterized by comprising the following steps of: adding the glucosamine hydrochloride and the glucosamine potassium / sodium sulfate according to the mol ratio of 2: 0.95 to 2: 1, adding 1500-3000ml of pure water every two mol of glucosamine hydrochloride, heating to 50 to 70 DEG C, stirring for 0.5 to 2h under the condition of preserving the temperature ; cooling to 20 to 40 DEG C, filtering, concentrating in vacuum under the condition of controlling the temperature at 50 to 70 DGE C until a great deal of crystals appear, stopping heating and concentrating, adding 1000 to 2000ml of 95% alcohol, standing for 4-24h, centrifuging and removing mother solution, crystallizing and drying to obtain the product. The technology has the advantages of simple and convenient operation, low cost, complete reaction of potassium / sodium salts, and the like.

Description

Technical field [0001] The invention relates to a co-crystallization technology, and specifically discloses a co-crystallization technology of glucosamine hydrochloride and glucosamine sulfate potassium salt / glucosamine sodium sulfate sodium salt. technical background [0002] Glucosamine Hydrochloride (Glucosamine Hydrochloride) can be produced by hydrolysis of chitin with hydrochloric acid. It is widely used and is the main raw material for the synthesis of anti-cancer drug chlorcarbamide and the latest third-generation functional health food additive. It can be used as an anti-bacterial infection, immune adjuvant, and an activator of the human body against influenza virus. It can promote the synthesis of chondrocyte proteoglycan, improve the viscosity of joint synovial fluid, improve the metabolism of articular cartilage, and effectively treat rheumatoid arthritis. [0003] Glucosamine sulfate potassium chloride is formed by the reaction of glucosamine sulfate and potassium su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H5/06C07H1/06C30B29/54
Inventor 周京石曹礼群魏献忠蒋永红张艳王行义赵全生
Owner 技源生物制品(徐州)有限公司