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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

Active Publication Date: 2008-07-02
JK SUCRALOSE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of this method are: the crystallization time is too long, which usually takes several days; the crystallization is not complete, and the crystallization mother liquor often contains a large amount of product, and the recovery of the mother liquor is cumbersome; the moisture content in the product is high, which affects the stability of the product
US5498709 mentions that ethyl acetate is used as a crystallization solvent to crystallize sucralose, but there are also problems of long crystallization time and low primary yield
US6943248 describes a method for crystallization with a mixed solvent of methanol and ethyl acetate, but because the boiling points of the two are too close, simple distillation equipment is difficult to achieve the purpose of separating methanol and forming crystals in ethyl acetate. In the patent, an evaporating tube is used to separate the two, but the product may be precipitated in the pipeline by using this device, which makes it difficult to continue further production, but it is obviously not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention discloses a crystallization method of trichloro sucrose. The method dissolves a concentrate or a solid that contains the trichloro sucrose in a mixed impregnant. The mixed impregnant contains two impregnant with large difference in boiling points; wherein, the impregnant with a low boiling point has higher solubility to the trichloro sucrose while the impregnant with a high boiling point has lower solubility to the trichloro sucrose. In the condition of proper temperature and vacuum degree, the impregnant is concentrated and crystals of the trichloro sucrose are separated when the impregnant with low boiling point volatilizes and finished product of trichloro sucrose crystals is obtained through filtering and desiccation after being settled. The method has the advantages of low production cost, high production yield, mild condition, stable quality and simple equipment, etc.

Description

technical field [0001] The present invention relates to a crystallization method of sucralose. Background technique [0002] Sucralose is a new type of sweetener, and sucralose is a kind of chlorinated sucrose. Its sweetness is 600 times that of sucrose. It does not participate in human metabolism, has high safety and strong ability to resist acid hydrolysis. These advantages make it the hottest strong sweetener on the market, and it has been approved for use by more than 30 countries. . US 4343934, US 5141860, US4977254, US4783526, US 4380476, US5298611 and other patents describe a crystallization method of sucralose: crystallization using water as a solvent. However, the disadvantages of this method are: the crystallization time is too long, which usually takes several days; the crystallization is incomplete, and the crystallization mother liquor often contains a large amount of product, and the recovery of the mother liquor is cumbersome; the moisture content in the pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/02C07H1/06
CPCA23L27/37C07H3/04C13B30/02
Inventor 王非何海兵余永柱范枝松杨欣
Owner JK SUCRALOSE
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