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Method for continuously synthesizing sucralose

A technology of sucralose and acetate, which is applied in the direction of chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of high content of impurities such as sucralose, affecting product purity, and difficulty in continuing the reaction. Achieve the effect of realizing automatic production, shortening the reaction time and stabilizing the reaction process

Pending Publication Date: 2021-06-22
FUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In addition, because the conventional reaction is carried out under the condition that the sucralose-6-ester is not dehydrated, the non-dehydrated sucralose-6-ester enters the reaction system, and after a long period of reaction, the water will be in the bottom of the tower. Enrichment leads to hydrolysis side reaction in the transesterification process to produce sodium acetate, leading to deactivation of the catalyst and difficulty in continuing the reaction
If the amount of catalyst is increased, the formation of by-products will continue to be promoted after the reaction reaches equilibrium, resulting in higher content of impurities such as sucralose, which will affect the purity of the product
Therefore, the existing transesterification process has problems such as catalyst deactivation, poor quality, low production efficiency, large energy consumption and high production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put a three-necked flask equipped with a packing tower, a water separator, and a vacuum pump in an oil bath, add 500ml of ethyl acetate and 100g of sucralose-6-acetate, and heat up to 60°C to dissolve. Then use a vacuum pump to adjust the system pressure to 60kPa, continue to heat up to 75°C, and reflux to separate water (every 2h, remove the water phase in the water separator) until there is no more water layer in the water separator. Add a receiving bottle at the outlet of the water separator, adjust the system pressure to 25~50kPa, and evaporate the ethyl acetate to the receiving bottle. A yellow viscous substance, namely dehydrated sucralose-6-acetate, was obtained.

Embodiment 2

[0026] Add 350 g of methanol to a three-necked flask containing 200 g of dehydrated sucralose-6-acetate, and heat to dissolve. Then the solution is transported to the feed port of the middle section of the rectification tower through the feed pump, and the feed flow rate is 1.5ml / min; Distillation tower, make sucralose-6-ester and NaOH mix in the tower and then react. The pressure at the top of the tower is 30kPa, the temperature is 32°C, and the mixture of methanol and methyl acetate is produced at the top of the tower according to the reflux ratio of 10:1. The temperature of the tower kettle is 45°C. The methanol solution of sucralose was extracted from the tower kettle, and the content of methyl acetate was 0.2%. After the solution in the tower kettle was acidified, acetic acid was not detected by GC analysis. According to liquid chromatography analysis, the conversion rate of sucralose-6-ethyl ester was 99.5%, the purity of sucralose was 99.7%, and the content of sucral...

Embodiment 3

[0028] Add 400 g of methanol to a three-necked flask containing 200 g of dehydrated sucralose-6-acetate, and heat to dissolve. Then the solution is transported to the feed port of the middle section of the rectification tower through the feed pump, and the feed flow rate is 2.5ml / min; Distillation tower, make sucralose-6-ester and NaOH mix in the tower and then react. The pressure at the top of the tower is 40kPa, the temperature is 35°C, and the mixture of methanol and methyl acetate is produced at the top of the tower according to the reflux ratio of 5:1. The temperature of the tower kettle is 55°C. The methanol solution of sucralose was extracted from the tower kettle, and the content of methyl acetate was 0.2%. After the solution in the tower kettle was acidified, acetic acid was not detected by GC analysis. According to liquid chromatography analysis, the conversion rate of sucralose-6-ethyl ester was 99.8%, the purity of sucralose was 99.6%, and the content of sucralo...

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Abstract

The invention discloses a method for continuously synthesizing sucralose, which comprises the following step: in the presence of a catalyst, reacting dehydrated sucralose-6-acetate and anhydrous low-carbon alcohol serving as raw materials in a reactive distillation tower to generate sucralose, wherein the dehydrated sucralose-6-ester and the anhydrous low-carbon alcohol are used as raw materials, so that the problem that the catalyst is inactivated due to the fact that sodium acetate is generated by hydrolysis in the transesterification process caused by water in the raw materials is solved; and the ester exchange reaction and the methyl acetate separation process are combined in one device, and the product methyl acetate is timely moved out of the reaction zone from the tower top during the ester exchange reaction, so that the reaction can be promoted. The method makes full use of the advantages of the reactive distillation column, can effectively improve the reaction conversion rate and the equipment efficiency, reduces the energy consumption, reduces the production cost, and has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of sucralose preparation, in particular to a method for continuously preparing sucralose from dehydrated sucralose-6-ester. Background technique [0002] As a high-quality functional sweetener, sucralose has gradually entered people's daily life. Adding a small amount of sucralose to some functional drinks can reach 600 times the sweetness of the same equivalent of ordinary sucrose, and it is not absorbed by the human body, and the calorie value is almost zero. Man brings the gospel. Sucralose, also known as 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose, is known for its good chemical stability, thermal stability and safe and healthy biological characteristics. It is widely used in industries such as food and pharmaceutical products, and its market demand is increasing day by day, making it highly valued in the global market, and its market development has attracted much attention. [0003] In the prev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H5/02
CPCC07H1/00C07H5/02Y02P20/10
Inventor 郑辉东苏晨欣周守泉陈小平庄浚杰
Owner FUZHOU UNIV
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