Preparation method of synthesized D-glucosamine sulfate sodium
A technology of glucosamine sulfate sodium salt and reactor is applied in the field of preparation of synthetic D-glucosamine sulfate sodium salt, and can solve the problems of different material densities of glucosamine sulfate sodium salt, unstable glucosamine sulfate, poor uniformity and the like , to achieve the effect of high purity, less impurities and low cost
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Embodiment 1
[0011] A preparation method for synthesizing D-glucosamine sulfate sodium salt, comprising the following steps:
[0012] A. Dissolution: Add water into the reactor, heat to 70°C, add sodium sulfate under stirring condition, after it dissolves, lower the temperature to 60°C, add D-glucosamine hydrochloride, continue stirring, wait After it dissolves, raise the temperature of the solution to 65°C, add an organic solvent, cool down to 15°C, and continue to stir for 10 hours, so that all materials are fully reacted in the reactor;
[0013] B. Crystallization: cool down the above-mentioned reacted materials to 0°C, crystallize under stirring conditions for 90 minutes, and then centrifuge and dehydrate in a centrifuge to obtain white crystals;
[0014] C. Drying: drying the centrifuged white crystals under vacuum at a temperature of 55° C. to obtain synthetic D-glucosamine sulfate sodium salt.
Embodiment 2
[0016] A preparation method for synthesizing D-glucosamine sulfate sodium salt, comprising the following steps:
[0017] A. Dissolution: Add water into the reactor, heat to 80°C, add sodium sulfate under stirring condition, after it dissolves, lower the temperature to 65°C, add D-glucosamine hydrochloride, continue stirring, wait After it dissolves, raise the temperature of the solution to 75°C, add an organic solvent, cool down to 25°C, and continue stirring for 15 hours, so that all materials are fully reacted in the reactor;
[0018] B. Crystallization: Cool down the above-mentioned reacted materials to -10°C, crystallize under stirring conditions for 120 minutes, and then centrifuge and dehydrate in a centrifuge to obtain white crystals;
[0019] C. Drying: drying the centrifuged white crystals under vacuum at a temperature of 65° C. to obtain synthetic D-glucosamine sulfate sodium salt.
Embodiment 3
[0021] A preparation method for synthesizing D-glucosamine sulfate sodium salt, comprising the following steps:
[0022] A. Dissolution: Add water into the reactor, heat to 75°C, add sodium sulfate under stirring condition, after it dissolves, lower the temperature to 62°C, add D-glucosamine hydrochloride, continue stirring, wait After it dissolves, the temperature of the solution is raised to 70°C, an organic solvent is added, the temperature is lowered to 20°C, and stirring is continued for 12 hours, so that all materials are fully reacted in the reactor;
[0023] B. Crystallization: Cool down the above-mentioned reacted materials to -5°C, crystallize under stirring conditions for 105 minutes, and then centrifuge and dehydrate in a centrifuge to obtain white crystals;
[0024] C. Drying: drying the centrifuged white crystals under vacuum at a temperature of 60° C. to obtain synthetic D-glucosamine sulfate sodium salt.
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