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
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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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