Preparation method for glucosamine sulfate

A technology of glucosamine sulfate and glucosamine, which is applied in the field of preparation of glucosamine sulfate, can solve the problems of corrosion reaction kettles, high requirements for organic membranes, and easy damage, so as to reduce environmental damage, stabilize product quality, and be easy to control Effect

Active Publication Date: 2015-06-17
迪嘉药业集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has high requirements on the organic membrane, and it is easily damaged. A large amount of concentrated sulfuric acid in the production will corrode the reactor, and a large amount of waste liquid produced by the reaction has caused great environmental pollution.

Method used

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  • Preparation method for glucosamine sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 Weigh 100g of D-glucosamine hydrochloride and add it to 1L of 80% ethanol. The reaction process has been under the protection of nitrogen. Dissolve 27.8g of sodium hydroxide in a small amount of water and add it to the above solution. Stir, control the temperature at 50 °C, and react for 4 hours; slowly add sulfuric acid with a concentration of 50% to the D-glucosamine solution for reaction, control the final pH value of the solution at 3.0, and leave it for 30 minutes without changing the pH value. The mixture was stirred for 9 hours, and the temperature was controlled at 25° C.; after the reaction was completed, 1 L of acetone was added to the solution, and after standing for 3 hours, the reaction solution after the reaction was filtered. And the filtered solid glucosamine sulfate was soaked in 300ml 80% ethanol for 0.5h, stirred properly during soaking, and then filtered, and the solid was washed repeatedly with 80% ethanol until no chloride ions were wash...

Embodiment 2

[0025] Example 2 Weigh 100g of D-glucosamine hydrochloride and add it to 800mL of 90% ethanol. The reaction process has been under the protection of nitrogen. Take 38.96g of potassium hydroxide and dissolve it in a small amount of water, add it to the above solution, and keep stirring , control the temperature at 40°C, and react for 6 hours; after the reaction, slowly add sulfuric acid with a concentration of 40% to the D-glucosamine solution for reaction, control the final pH value of the solution to 5.0, leave it for 30 minutes without changing the pH value, stir for 2 hours, The reaction temperature was controlled at 50° C.; after the reaction was completed, 800 mL of acetone was added to the solution, and after standing for 4 hours, the reaction solution after the reaction was filtered. Soak the filtered solid glucosamine sulfate in 200 mL of 80% ethanol for 1 hour, stir properly during soaking, then filter, and wash the solid repeatedly with 80% ethanol until no chloride...

Embodiment 3

[0026] Example 3 Weigh 100g of D-glucosamine hydrochloride and add it to 500 mL of 90% propanol. The reaction process has been under the protection of carbon dioxide gas. Dissolve 22.3g of sodium hydroxide in a small amount of water and add it to the above solution , keep stirring, control the temperature at 10°C, and react for 10 hours; after the reaction is over, slowly add sulfuric acid with a concentration of 35% to the D-glucosamine solution for reaction, adjust the pH value of the solution to 6.0, leave it for 30 minutes without changing the pH value, and stir After 10 hours, the reaction temperature was controlled at 10°C; after the salt formation was completed, 1200 mL of acetone was added to the solution, and after standing for 5 hours, the reaction solution after the reaction was filtered. Soak the filtered solid glucosamine sulfate in 300 mL of 90% ethanol for 5 hours, stir properly during soaking, and then filter. Repeat this step until no chloride ions are washed...

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Abstract

The invention relates to a preparation method for glucosamine sulfate. According to a technical scheme in the invention, the preparation method comprises the following steps: step 1, dispersing D-glucosamine hydrochloride in an alcoholic solvent; step 2, neutralizing D-glucosamine hydrochloride with alkali; step 3, adding sulfuric acid into a glucosamine solution drop by drop so as to form a salt; step 4, carrying out precipitation and separation; and step 5, carrying out refining by repeatedly washing a solid with a small amount of an organic solvent until no chloride ion is eluted and carrying out drying under reduced pressure, wherein the organic reagent is ethanol, propyl alcohol, acetone or the like with a concentration of 80 to 100%. With the technical scheme, glucosamine sulfate with low sodium or potassium content is obtained.

Description

technical field [0001] The invention relates to a preparation method of glucosamine sulfate. Background technique [0002] Glucosamine is a natural amino monosaccharide, and it is an essential component of human connective tissue and cell membrane. Both the respiratory system and the urinary system have important effects on the production of mucus secretions, and are specific substrates for the production of amino polysaccharides and proteoglycans in the human body. Glucosamine sulfate can obviously relieve the pain of arthritis and rheumatism patients and improve, prevent, treat and repair connective tissue damage. Heart disease, pneumonia also have a certain effect. [0003] Commercially available glucosamine sulfate is a balanced product of glucosamine hydrochloride and sodium (potassium) sulfate. It is directly mixed with glucosamine hydrochloride and sodium (potassium sulfate), or dissolved in water and then dried to obtain its double salt. The product It contains ab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/06C07H1/00
Inventor 李广生夏文水邵先祥
Owner 迪嘉药业集团股份有限公司
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