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Preparation method for sulphuric acid glucosamine

A technology of glucosamine sulfate and sulfuric acid is applied in the field of compounds containing amino sugars, which can solve problems such as production safety and environmental problems, and achieve the effects of less environmental pollution, safe production process, and clean production process.

Active Publication Date: 2009-01-14
厦门蓝湾科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the technology involved in this method requires the use of a large amount of organic solvents, and the removal of excess sulfuric acid by alkali precipitation will produce a large amount of calcium sulfate or barium sulfate precipitation, and the production of one ton of glucosamine sulfate will produce more than one ton of calcium sulfate or barium sulfate Waste slag, causing production safety and environmental problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 20g of chitin, add 40g of sulfuric acid with a mass concentration of 90%, and cool it in an ice bath to about 0°C. After degrading at this temperature for 8 hours, slowly add deionized water to dilute the reaction liquid system until the acidity reaches 8%, and heat up to 110°C. ℃, maintain this temperature range to continue the reaction for 4 hours, and filter to obtain a brown solution. Diffusion dialysis is used to remove sulfuric acid until the mass concentration of sulfuric acid is below 5%, and the nanofiltration membrane with a molecular weight cutoff of 150 Daltons is used to remove sulfuric acid until the pH value of the solution is 5.8. The resulting solution was concentrated to a mass concentration of 10% with a vacuum concentrator. The concentrate is dried by centrifugal spraying to obtain glucosamine sulfate without sodium, potassium and chlorine, and the yield is 41.2%.

Embodiment 2

[0027] Weigh 20g of chitin, add 44g of sulfuric acid with a mass concentration of 80%, and cool in a cold water bath. After 11 hours of degradation reaction at this temperature, continue the reaction at 50°C for 1 hour, and then slowly add deionized water to dilute the reaction liquid system until the acidity reaches 1%. Raise the temperature to 60° C., maintain this temperature range and continue the reaction for 2 hours, and filter to obtain a brown solution. Diffusion dialysis is used to remove sulfuric acid until the mass concentration of sulfuric acid is below 5%, and the nanofiltration membrane with a molecular weight cut-off of 400 Daltons is used to remove sulfuric acid until the pH of the solution is 6.0. The resulting solution was concentrated to a mass concentration of about 30% with a vacuum concentrator. The concentrated solution is freeze-dried to obtain glucosamine sulfate without sodium, potassium and chlorine, and the yield is 47.5%.

Embodiment 3

[0029] Weigh 20g of chitin, add 48g of sulfuric acid with a mass concentration of 70%, and after 15h of degradation reaction at room temperature, continue the reaction at 50°C for 1h, then slowly add deionized water to dilute the reaction solution until the acidity reaches 15%, and heat up to 80°C. Maintain this temperature range to continue the reaction for 5 hours, and filter to obtain a brown solution. Diffusion dialysis is used to remove sulfuric acid until the mass concentration of sulfuric acid is below 5%, and the nanofiltration membrane with a molecular weight cutoff of 350 Daltons is used to remove sulfuric acid until the pH of the solution is 6.2. The resulting solution was concentrated to a mass concentration of about 40% with a vacuum concentrator. The concentrated solution is freeze-dried to obtain glucosamine sulfate without sodium, potassium and chlorine, and the yield is 53.2%.

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Abstract

The invention discloses a preparation method of glucosamine sulfate, relating to a compound containing aminosugar. The preparation method of glucosamine sulfate has the advantages that a great deal of sulfate precipitation by-product is avoided being generated and a great deal of organic solvent is avoided being used, the operation is in complete aqueous phase, the production processes are safe, the sulfuric acid removed by the membrane method can be recovered and used, the production cost is reduced, exhaust and waste residue are not produced, the prepared product does not contain sodium, potassium or chlorine, the purity of the product reaches over 95 percent, and the glucosamine sulfate can be used to treat osteoarthritis without usage taboo. The preparation method is characterized in that chitin is adopted as the raw material, and a degradation agent of concentrated sulfuric acid is used to cause the chitin to generate degradation reaction; diluted sulfuric acid is used as a deacetylation agent to cause the degraded chitin to generate deacetylation reaction; the chitin which is not reacted after the deacetylation reaction is filtered, and the unreacted sulfuric acid is removed by the membrane method; and the solution, in which the unreacted sulfuric acid is removed, is decolorized, concentrated and dried, and glucosamine sulfate is obtained.

Description

technical field [0001] The invention relates to a compound containing amino sugars, in particular to a preparation method of glucosamine sulfate. Background technique [0002] Serious imbalance of proteoglycan metabolism, increased expression of inflammatory factors and α-tumor necrosis factor, activation of matrix metalloproteinases and nitric oxide synthase, prostaglandin E 2 Osteoarticular cartilage degeneration, leading to joint structure destruction and progressive functional degeneration, commonly known as osteoarthritis. For a long time, fast-acting drugs that improve symptoms have been commonly used in the treatment of osteoarthritis, including painkillers, non-steroidal anti-inflammatory drugs, and glucocorticoids. These drugs mainly achieve the purpose of anti-inflammatory and pain relief by inhibiting cyclooxygenase in damaged tissues and reducing the synthesis of prostaglandins. However, long-term use of painkillers, non-steroidal anti-inflammatory drugs, and g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/06A61P19/02
Inventor 林秀芬孙丽石国宗
Owner 厦门蓝湾科技有限公司
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