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Method for increasing crystallization yield of trichloro sucrose-6-acetate

A sucralose and crystallization technology, applied in the field of increasing the crystallization yield of sucralose-6-ethyl ester, can solve problems such as difficulty in crystallization solvent recovery, poor safety, etc., and achieve reduced product cost, increased crystallization yield, and good purity Effect

Inactive Publication Date: 2018-07-06
SHANDONG KANBO BIOCHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN201210259307.4 reports a method for crystallizing sucralose-6-ethyl ester using a mixed solution of methyl acetate-propane (or methyl acetate-butane), but since propane or butane is Flammable and explosive gas, which is easily volatilized from the crystallization system, the corresponding process is not only poor in safety, but also very difficult to recover the crystallization solvent

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  • Method for increasing crystallization yield of trichloro sucrose-6-acetate

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Embodiment 1

[0011] Embodiment 1: A method for improving the crystallization yield of sucralose-6-ethyl ester mentioned in the present invention comprises the following steps:

[0012] At room temperature, add 30.0 g of crude sucralose-6-ethyl ester (purity 89.0%), 20.0 g of methanol, and 20.0 g of n-hexane into a 100 ml three-necked flask, then raise the temperature to 60°C and stir at this temperature for 1 hour, then Stir at low speed and cool down to room temperature naturally, then cool the above solution to 0°C and let it stand for crystallization for 3 hours, finally filter and dry to obtain 27.6g of sucralose-6-ethyl ester crystals (crystallization yield 92.0%, liquid chromatography detection The purity is 98.5%. The present invention significantly improves the crystallization yield and reduces the product cost under the premise of ensuring the product purity).

Embodiment 2

[0013] Embodiment 2: A method for improving the crystallization yield of sucralose-6-ethyl ester mentioned in the present invention comprises the following steps:

[0014] At room temperature, add 30.0 g of crude sucralose-6-ethyl ester (purity 89.0%), 20.0 g of ethanol, and 20.0 g of n-hexane into a 100 ml three-necked flask, then raise the temperature to 60°C and stir at this temperature for 1 hour, then Stir at low speed and naturally cool down to room temperature, then cool the above solution to 10°C and let it stand for crystallization for 3 hours, finally filter and dry to obtain 26.0 g of sucralose-6-ethyl ester crystals (crystallization yield 86.7%, liquid chromatography detection The purity is 99.3%).

Embodiment 3

[0016] At room temperature, add 30.0g of crude sucralose-6-ethyl ester (purity 89.0%), 20.0g of propanol, and 20.0g of n-hexane into a 100ml three-necked flask, then raise the temperature to 60°C and stir at this temperature for 1 hour. Then stir at low speed and naturally cool down to room temperature, then cool the above solution to -10°C and let it stand for crystallization for 3 hours, finally filter and dry to obtain 28.6g of sucralose-6-ethyl ester crystals (95.3% crystallization yield, liquid phase Chromatographically detected purity was 95.7%).

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Abstract

The invention relates to a method for increasing the crystallization yield of trichloro sucrose-6-acetate. The method is characterized by comprising the following production steps: mixing 30.0 parts of a trichloro sucrose-6-acetate crude product with 40.0 parts of a crystallization solvent according to a proportion at room temperature, and adding the obtained mixture into a reaction kettle; then,heating up to 50-70 DEG C and stirring for 1h at the temperature of 50-70 DEG C; after that, stirring at low speed, naturally cooling to room temperature, then cooling the solution to -10 to 10 DEG C,standing and crystallizing for 3h; finally, filtering and drying to obtain the trichloro sucrose-6-acetate crystals. The method has the beneficial effects that a mixed solvent formed by alcohol and alkane is used as a crystallization solvent, and crystallization is performed at the low temperature of -10 to 10 DEG C, so that the product yield is high, and the product purity is good; the mixed solvent used in the method is better in solubility to the trichloro sucrose-6-acetate at the high temperature and poorer in solubility to the trichloro sucrose-6-acetate at the low temperature, so that the dissolution of impurities and the precipitation of the product are facilitated. The method obviously increases the crystallization yield and lowers the product cost under the premise of guaranteeing the product purity.

Description

technical field [0001] The invention relates to a method for purifying a sweetener intermediate, in particular to a method for increasing the crystallization yield of sucralose-6-ethyl ester. Background technique [0002] Sucralose (CAS No.: 56038-13-2) is a new type of sweetener, which has the advantages of high sweetness (about 600 times that of sucrose), easily soluble in water, low calorie, and hardly absorbed by the human body. , the market prospect is very broad. At present, the method of industrially synthesizing sucralose is as follows: using sucrose as raw material, sucrose is subjected to esterification reaction to obtain sucrose-6-ethyl ester, and then chlorinated sucrose-6-ethyl ester to obtain sucralose-6-ethyl ester , and finally degreasing sucralose-6-ethyl ester to obtain sucralose. [0003] In the three steps of producing sucralose in the existing process, the chlorination reaction selectivity of sucralose-6-ethyl ester prepared by chlorination of sucralos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/06
CPCC07H1/06C07H13/06
Inventor 胡兴邦李建新李建彬吴有庭徐松波
Owner SHANDONG KANBO BIOCHEM TECH
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