Crystallization method for trichlorosucrose
一种三氯蔗糖、结晶的技术,应用在三氯蔗糖结晶领域,能够解决结晶时间长、一次收率低、结晶不完全等问题,达到结晶时间短、操作简单、设备简单的效果
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Embodiment 1
[0020] Sucralose-6-ethyl ester (content 99.0%) 20g, deacylation reaction to obtain sucralose (100ml methanol solution), concentrate the solution to 40ml, add n-butanol 80ml, keep the temperature of the water bath at about 40C, in a vacuum of - The methanol was evaporated under reduced pressure at about 0.095Mpa, and after standing for a period of time, crystals precipitated out of the solution. Continue to concentrate until no methanol is evaporated, lower the temperature of the solution to 5° C. and let it stand for 5 hours, filter, and dry in vacuum to obtain 14.3 g of finished sucralose (content 99.1%).
Embodiment 2
[0022] Sucralose-6-ethyl ester (content 99.0%) 20g, obtained sucralose (100ml methanol solution) through deacylation reaction, concentrated to dryness, after adding 30ml of acetonitrile to dissolve, after adding 80ml of amyl acetate and stirring evenly, in vacuum The acetonitrile was evaporated under reduced pressure at about -0.095Mpa, and after standing for a period of time, crystals were precipitated in the solution. Continue to concentrate until no acetonitrile evaporates, lower the temperature of the solution to 10° C. and let it stand for 5 hours, filter, and dry in vacuo to obtain 15.7 g of finished sucralose (content 98.9%).
Embodiment 3
[0024] Dissolve 20 g of sucralose (content 99.1%) obtained by the method described in Example 1 in 50 ml of methanol, add 70 ml of isobutanol, stir evenly, evaporate methanol under reduced pressure at a vacuum degree of about -0.095 Mpa, and let stand for a period of time Afterwards, crystals precipitated out of the solution. Concentration was continued until no methanol was evaporated, the temperature of the solution was lowered to 10° C. and left to stand for 5 hours, filtered, and vacuum-dried to obtain 16.3 g of finished sucralose (content 99.5%).
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