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Preparation method of catalyst organotin acetate in sucralose production

A technology of sucralose and organotin, which is applied to the preparation of sugar derivatives, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of solvent volatilization, high energy consumption, and long preparation time, and achieve improved production efficiency , The process is simple and the effect of reducing production costs

Inactive Publication Date: 2020-08-28
ANHUI JINGHE IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of solvent volatilization, high energy consumption and long preparation time in the existing preparation method of organotin acetate (DSDA), and provide organotin acetate (DSDA) in the production of sucralose preparation method

Method used

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  • Preparation method of catalyst organotin acetate in sucralose production

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Add 100g of dibutyltin diacetate liquid into a 500ml three-necked flask, start stirring, raise the temperature to 80°C, slowly add 70g of dibutyltin oxide into the three-necked flask, and finish adding in about 30 minutes.

[0029] 2. After the addition of dibutyltin oxide, raise the temperature to 100°C and start to heat and dissolve for 3 hours. After the dissolution is complete, heat for half an hour and cool down to 80°C.

[0030] 3. Distill the reacted liquid under reduced pressure at -0.95MPa and 80°C until no components are distilled out, and the reaction is over. 176.8 g of organotin acetate can be obtained. It is solid at room temperature and liquid above 60°C.

[0031] 4. Finally, the prepared organotin acetate (DSDA) is used as a catalyst, and returns to the esterification section to participate in the esterification reaction for reuse.

Embodiment 2

[0033] 1. Add 100g of dibutyltin diacetate liquid into a 500ml three-necked flask, start stirring, raise the temperature to 60°C, slowly add 82g of dibutyltin oxide into the three-necked flask, and finish adding in about 2 hours.

[0034] 2. After adding dibutyltin oxide, raise the temperature to 70°C and start to keep warm and dissolve for 4 hours. After the dissolution is complete, keep warm for half an hour, and then cool down to 60°C.

[0035] 3. Distill the reacted liquid under reduced pressure at -0.95MPa, 60°C until no components are distilled out, and the reaction is over. 177.1 g of organotin acetate can be obtained. It is solid at room temperature and liquid above 60°C.

[0036] 4. Finally, the prepared organotin acetate (DSDA) is used as a catalyst, and returns to the esterification section to participate in the esterification reaction for reuse.

Embodiment 3

[0038] 1. Add 100g of dibutyltin diacetate liquid into a 500ml three-necked flask, start stirring, raise the temperature to 100°C, slowly add 70g of dibutyltin oxide into the three-necked flask, and finish adding in about 60 minutes.

[0039] 2. After adding dibutyltin oxide, heat it at 100°C for 2 hours to dissolve. After the dissolution is complete, heat it for half an hour and cool down to 80°C.

[0040] 3. Distill the reacted liquid under reduced pressure at -0.95MPa, 80°C until no components are distilled out, and the reaction is over. 176.9 g of organotin acetate can be obtained. It is solid at room temperature and liquid above 60°C.

[0041] 4. Finally, the prepared organotin acetate (DSDA) is used as a catalyst, and returns to the esterification section to participate in the esterification reaction for reuse.

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Abstract

The invention relates to a preparation method of a catalyst organotin acetate (DSDA) in sucralose production. The method comprises the following steps: directly reacting dibutyltin diacetate and dibutyltin oxide at a certain temperature to obtain organotin acetate (DSDA), and distilling the reacted material under reduced pressure to remove impurities, thereby obtaining the organotin acetate (DSDA)which can be used in sucralose esterification reaction. The method is simple and smooth in process, and can basically realize one-step implementation. And under the same equipment condition, the production efficiency is greatly improved. The problems of solvent volatilization and high energy consumption in the prior art are solved, and the solvent and steam consumption is reduced; and the environment is protected, the working intensity of field operators is greatly reduced, and the working environment is improved.

Description

technical field [0001] The invention belongs to the technical field of food additive production, and in particular relates to a method for preparing a catalyst organotin acetate for sucralose production. Background technique [0002] Sucralose, first synthesized by the British company Tate & Lyte, can reach about 600 times the sweetness of sucrose. Sucralose is characterized by no energy, high sweetness, pure sweetness, and high safety. It is also one of the most competitive sweeteners synthesized so far. [0003] Sucrose-6-acetate is an important intermediate in the synthesis of sucralose. Currently, its production process mainly uses 1,3-diacetoxy-1,1,3,3-tetrabutyldistannoxane (DSDA) As a reaction catalyst, the preparation of catalyst organotin acetate (DSDA) in the more general sucralose production process is mainly through the following process: dibutyltin oxide solid is dispersed in a solvent and then acetic anhydride is added dropwise (CN 109651428 A ) or acetic aci...

Claims

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Application Information

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IPC IPC(8): C07F7/22B01J31/12C07H5/02C07H1/00
CPCC07F7/2224C07F7/2296B01J31/12C07H5/02C07H1/00B01J2231/49
Inventor 梁金俊沈东东吕祖鹏刘学立
Owner ANHUI JINGHE IND
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