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Preparation method of glucosamine sulfate and sodium chloride double salt

A technology of glucosamine sulfate and sodium chloride is applied in the field of medicine and chemical industry, and can solve the problems of low concentration of glucosamine, easy moisture absorption of finished products, high production difficulty, etc., and achieve the effects of simple process, improved product yield and high product quality.

Active Publication Date: 2017-05-31
GUANGDONG XIANQIANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is cumbersome, a large amount of water is produced after ion resin exchange, the concentration of glucosamine is low, and it needs to be concentrated or freeze-dried after salt formation, high cost, low quality, and difficult production
In addition, the activation and regeneration of the resin will also generate a large amount of waste water.
[0009] In summary, the current preparation method of glucosamine sulfate sodium chloride double salt has complex processes, high cost, unstable quality, easy moisture absorption of finished products, and problems such as discoloration

Method used

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  • Preparation method of glucosamine sulfate and sodium chloride double salt
  • Preparation method of glucosamine sulfate and sodium chloride double salt
  • Preparation method of glucosamine sulfate and sodium chloride double salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The Effect of Sodium Chloride on the Hydrolysis of Chitin

[0050] plan 1:

[0051] Add 100g of chitin and 600mL of 60% sulfuric acid into the three-neck flask, raise the temperature to 55°C, keep the temperature for 4h, do not add sodium chloride as a stabilizer, continue to heat up to 70°C for 1h, and then quickly drop the reaction solution to 50°C, then At this time, about 5% of chitin was still unreacted and dissolved, and 10 g of activated carbon and 15 g of diatomaceous earth were added to decolorize for 0.5 h. Pad diatomaceous earth to filter, measure the amount of glucosamine sulfate and the situation of related substances in the filtrate.

[0052] Scenario 2:

[0053] Add 100g of chitin and 600mL of 60% sulfuric acid into the three-neck flask, raise the temperature to 55°C, keep the temperature for 4h, add 10g of sodium chloride as a stabilizer, continue to heat up to 70°C for 1h, then quickly drop the reaction solution to 50°C, then At this time, about 5% o...

Embodiment 2

[0063] Influence of one-time high temperature and gradient temperature rise on acid hydrolysis reaction

[0064] plan 1:

[0065] Add 100g of chitin and 500mL of 70% sulfuric acid into the three-neck flask, raise the temperature to 75°C, keep it warm for 6h, then quickly lower the reaction solution to 50°C, add 15g of activated carbon, 15g of diatomaceous earth, and decolorize for 0.5h. Pad diatomaceous earth to filter, measure the amount of glucosamine sulfate and the situation of related substances in the filtrate.

[0066] Scenario 2:

[0067] Add 100g of chitin and 500mL of 70% sulfuric acid into the three-neck flask, raise the temperature to 55°C, keep it warm for 4h, continue to heat up to 75°C for 2h, then quickly lower the reaction solution to 50°C, add 15g of activated carbon, 15g of diatomaceous earth, decolorize 0.5h. Pad diatomaceous earth to filter, measure the amount of glucosamine sulfate and the situation of related substances in the filtrate.

[0068] Opti...

Embodiment 3

[0075] Put 500g of chitin and 3.5kg of 50% sulfuric acid into the reaction kettle, heat up to 55°C, keep warm for 5h, add 100g of sodium chloride, continue to heat up to 70°C for 1.5h, and then quickly drop the reaction solution to 50°C, at this time , Chitin still has about 8% unreacted and dissolved, add 250g of activated carbon, 250g of diatomaceous earth, and decolorize for 0.5h. Pad Celite to filter, transfer the filtrate to another kettle, quantitatively add 50g of sodium chloride, heat up to 50°C, stir and dissolve until clear, keep warm for 1h, and then cool down to room temperature. Divide the feed solution into 10 equal parts, number from 1 to 10, add ethyl acetate, butyl acetate, dichloromethane, chloroform, methyl tert-butyl ether, diethyl ether, isopropyl ether, toluene, di 300mL each of 9 kinds of extractants such as toluene were extracted in 3 times, and the 10th group was the blank group. After the above 10 groups were extracted respectively, the aqueous phase...

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Abstract

The invention discloses a preparation method of glucosamine sulfate and sodium chloride double salt. The preparation method comprises the following steps: adding chitin and dilute sulfuric acid into a reactor, wherein the concentration of the dilute sulfuric acid is 40%-90%, and the mass ratio of the dilute sulfuric acid to the chitin is (3-10):1; performing a fist stage of temperature rise and thermal insulation reaction, wherein the temperature in the fist stage of temperature rise is 40-70 DEG C, and the time in the fist stage of thermal insulation is 2-10 hours; then adding sodium chloride as a reaction stabilizer, wherein the mass ratio of the sodium chloride to the chitin is (0.1-0.5):1; performing a second stage of temperature rise and thermal insulation reaction, wherein the temperature in the second stage of temperature rise is 70-90 DEG C, and the time in the fist stage of thermal insulation is 1-5 hours; after the completion of basic reaction, quickly reducing the temperature of reaction liquid. The preparation method disclosed by the invention is simple in process and low in cost, and facilitates industrial production; an obtained finished product is stable in property, difficult to yellow and moisten, and good in impurity situations; the contents of glucosamine sulphate and sodium chloride conform to the drug requirements; the quality is stable.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, in particular to a preparation method of glucosamine sulfate sodium chloride double salt. Background technique [0002] In 1956, Swedish researchers first discovered that glucosamine might play a role in the etiology of osteoarthritis. After decades of research and clinical trials by scientists from various countries, glucosamine has been widely used as the first choice for the treatment of osteoarthritis in the United States and European countries since the end of the 20th century. A large number of clinical studies have shown that the safety of glucosamine in the treatment of early and mid-term osteoarthritis is very good, which is reflected in the fact that there are very few adverse events during the medication process, and the patient's medication compliance is satisfactory. [0003] Glucosamine is a natural amino monosaccharide, which is an important component necessary for th...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00C07H1/06
Inventor 谭珍友刘斌罗统有刘道甫邓军程志伟
Owner GUANGDONG XIANQIANG PHARMA
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