Purification method of sucralose-6-ethyl ester

A technology of sucralose and purification method, which is applied in the direction of organic chemical methods, chemical instruments and methods, esterified saccharides, etc., and can solve the problems of poor crystallization efficiency of ethyl acetate, large amount of organic solvent used, and large solvent consumption, etc. problems, achieve the effect of reducing the number of crystallization times and the amount of organic solvent used, high single-pass crystallization yield and efficiency, and high product yield

Active Publication Date: 2021-04-09
ANHUI JINGHE IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN101328195 disclosed earlier the purification method of ethyl acetate and water recrystallization to extract sucralose-6-ethyl ester. This method is an earlier technology applied in industry at present. The single-pass yield is high, but the purity is low, and Requires multiple recrystallizations, high solvent consumption
However, the use of a single solvent is bound to be unable to effectively separate various by-products, thus causing problems such as poor crystallization efficiency of ethyl acetate in the current process, many crystallization times, and a large amount of organic solvents used.

Method used

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  • Purification method of sucralose-6-ethyl ester
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  • Purification method of sucralose-6-ethyl ester

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Add 1m into the first crystallization reactor E-1 3 , Ethyl acetate (purity greater than 99%, commercially available) high-temperature saturated solution of crude sucralose-6-ethyl ester at 60°C (the crude product of sucralose-6-ethyl ester obtained in the sucralose production process is dissolved in It is prepared from ethyl acetate solvent, its purity is detected by high performance liquid chromatography), the stirring rate is 10r / min, the temperature is lowered to 40°C, 50L of n-pentane (purity greater than 99%, commercially available) is added dropwise, and Add time for 5min, continue to stir and crystallize for 0.5h. After the crystallization is completed, the material is input into the first solid-liquid separator H-1 for separation, and the separated mother liquor enters the second crystallization reactor E-2, the temperature is lowered to 30°C, the stirring rate is 10r / min, and 100L of n-pentane is added dropwise , Dropping time 10min, continue to stir and crys...

Embodiment 2

[0058] Add 2m to the first crystallization reactor E-1 3 , ethyl acetate (purity greater than 99%, commercially available) high-temperature saturated solution of crude sucralose-6-ethyl ester at 70°C (the crude product of sucralose-6-ethyl ester obtained in the sucralose production process is dissolved in It is prepared from ethyl acetate solvent, and its purity is detected by high performance liquid chromatography), the stirring rate is 20r / min, the temperature is lowered to 50°C, 200L cyclopentane is added dropwise, the dropwise addition time is 20min, and the stirring and crystallization is continued for 40min; After the crystallization is completed, the material is input into the first solid-liquid separator H-1 for separation, and the separated mother liquor enters the second crystallization reactor E-2, the temperature is lowered to 20°C, the stirring rate is 15r / min, and 150L cyclopentane is added dropwise. Add dropwise for 15 minutes, continue to stir and crystallize f...

Embodiment 3

[0063] Add 1.5m to the first crystallization reactor E-1 3 , ethyl acetate (purity greater than 99%, commercially available) high-temperature saturated solution of crude sucralose-6-ethyl ester at 65°C (the crude product of sucralose-6-ethyl ester obtained in the sucralose production process is dissolved in It is prepared from ethyl acetate solvent, its purity is detected by high performance liquid chromatography), the stirring rate is 15r / min, the temperature is lowered to 45°C, 225L of n-hexane (purity greater than 99%, commercially available) is added dropwise, and The time is 20 minutes, continue to stir and crystallize for 45 minutes; after the crystallization is completed, the material is input into the first solid-liquid separator H-1 for separation, and the separated mother liquor enters the second crystallization reactor E-2, and the temperature is lowered to 25°C, and the stirring rate is 20r / min , add 80L of n-pentane dropwise, dropwise for 10min, continue to stir a...

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Abstract

The invention discloses a purification method of sucralose-6-ethyl ester. The purification method comprises the following steps: a preparation step: obtaining an ethyl acetate saturated solution of crude sucralose-6-ethyl ester heated to a preset temperature; a gradient crystallization step: cooling crystallizing and filtering the saturated solution for multiple times, dropwise adding a low-polarity solvent into the solution in each cooling crystallizing process to gradually reduce the polarity of the solution system during crystallizing, and collecting a sucralose-6-ethyl ester crude product obtained by multiple times of crystallization and filtration; and a purification step: recrystallizing and purifying the collected sucralose-6-ethyl ester crude product by using a mixed solution of ethyl acetate and a low-polarity solvent to obtain a sucralose-6-ethyl ester fine product with higher purity. On the basis of cooling crystallization of sucralose-6-ethyl ester by using ethyl acetate as an initial solvent, the polarity of the mixed solvent is reduced by gradually adding a low-polarity solvent, so that the effectiveness of impurity separation in each gradient stage is improved, the product yield is high, and the product quality is good.

Description

technical field [0001] The invention relates to the technical field of chemical purification, in particular to a method for purifying sucralose-6-ethyl ester. Background technique [0002] Sucralose-6-ethyl ester is one of the important intermediates in the production process of sucralose, and its purity is one of the keys affecting the yield of sucralose. According to research, when the purity of sucralose-6-ethyl ester is 80%, the yield of sucralose after deacylation is 45%; and when the purity is increased to 90%, the yield is correspondingly increased to 67%. Therefore, increasing the purity of sucralose-6-ethyl ester can effectively increase the yield of sucralose. At present, ethyl acetate, butyl acetate, and water are generally used in industry to purify sucralose-6-ethyl ester, and generally adopt multiple recrystallization methods. [0003] Currently there are patent reports on the purification of sucralose-6-ethyl ester. Chinese patent CN101328195 disclosed earl...

Claims

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Application Information

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IPC IPC(8): C07H13/04C07H1/06
CPCC07H13/04C07H1/06C07B2200/13Y02P20/10
Inventor 许传久徐成刚陈永乐
Owner ANHUI JINGHE IND
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