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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, incomplete reaction of potassium/sodium salt, complex process, etc.

Inactive Publication Date: 2010-06-16
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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0022] The obtained glucosamine sulfate sodium salt 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) of glucosamine hydrochloride, add 170.8g (0.98mol) of potassium sulfate, add 2000ml of pure water, heat to 60-65°C, keep stirring within this range for 1h; then cool to 30-35 ℃, filter with 0.22μm polypropylene membrane; at 50~70℃, concentrate under reduced pressure until a large number of crystals appear, stop heating and concentrate, add 1000ml of 95% ethanol, let it stand for 12h, centrifuge, crystallize and dry, and obtain 591.0g. The rate is 97.6%.

[0025] The obtained glucosamine sulfate potassium salt has a content of 99.3%, an optical rotation of +51.3°, a pH of 4.3, an ash content of 28.5%, and a moisture content of 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, specifically discloses a co-crystallization technology of glucosamine hydrochloride and glucosamine sulfate potassium salt / glucosamine sulfate sodium salt. technical background [0002] Glucosamine Hydrochloride can be produced by hydrolysis of chitin with hydrochloric acid. It is widely used, and it is the main raw material for the synthesis of anticancer drug chlorurecin, and it is the latest third-generation functional health food additive. It can be used as an anti-bacterial infection, an immune adjuvant, and an activator of human anti-influenza virus. It can promote the synthesis of chondrocyte proteoglycan, increase the viscosity of joint synovial fluid, improve the metabolism of articular cartilage, and effectively treat rheumatoid arthritis. [0003] Glucosamine sulfate potassium chloride is produced by the reaction of glucosamine hydrochloride and potassium sulfate. It has an auxilia...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/06C30B29/54
Inventor 周京石
Owner 技源生物制品(徐州)有限公司