Method for continuously preparing and supplementing organic tin catalyst in sucralose production

A sucralose and organotin technology, which is applied in the preparation of sugar derivatives, organic chemistry, chemical instruments and methods, etc., can solve the problems of large solvent and energy consumption, complicated preparation process, etc., and achieves saving production equipment and production costs, The effect of simplifying the process and improving the utilization rate

Inactive Publication Date: 2020-08-25
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the disadvantages of complex preparation process, large solvent and energy consumption of exist

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Pour 5,000 l of the cyclohexane phase containing organotin acetate after acylation extraction into the cyclohexane still, start stirring, and turn on the steam to raise the temperature to 50°C;

[0024] 2. Add 60kg of dibutyltin oxide into the reaction kettle, stir for 30 minutes, turn on the steam, start to heat up to 80°C, and keep the temperature for 3 hours;

[0025] 3. After the reaction is completed, lower the temperature to 50°C, distill off cyclohexane under reduced pressure, and the pressure condition is -0.090MPa. After the reaction, the organotin acetate (DSDA) can be weighed and detected to reach the initial input amount, and then returned to the system for esterification. After comparison after the esterification and acylation reaction, the yield of sucrose-6 ester obtained after the reaction of this method is 88-92%, which is compared with the yield of sucrose-6 ester obtained by the esterification and acylation operation of conventional newly added org...

Embodiment 2

[0031] 1. Pour 5,000 l of the cyclohexane phase containing organotin acetate after acylation extraction into the cyclohexane still, start stirring, and turn on the steam to raise the temperature to 60°C;

[0032] 2. Add 60kg of dibutyltin oxide into the reaction kettle, stir for 30 minutes, turn on the steam, start to heat up to 90°C, and keep the reaction for about 2 hours.

[0033] 3. After the reaction is completed, lower the temperature to 60°C, distill off cyclohexane under reduced pressure, and the pressure condition is -0.095MPa. After the reaction, the organotin acetate (DSDA) can be weighed and detected to reach the initial input amount, and then returned to the system for esterification. The yield of the sucrose-6 ester obtained after the reaction of the method is 88-92%, which is basically the same as the yield of the sucrose-6 ester obtained by the esterification and acylation operation with conventional newly added organotin.

Embodiment 3

[0035] 1. Pour 5,000 l of the cyclohexane phase containing organotin acetate after acylation extraction into the cyclohexane still, start stirring, and turn on the steam to raise the temperature to 70°C;

[0036] 2. Add 100kg of dibutyltin oxide into the reactor, stir for 30 minutes, turn on the steam, start to heat up to 90°C, and keep the reaction for about 5 hours.

[0037] 3. After the reaction is completed, lower the temperature to 50° C., and distill off cyclohexane under reduced pressure under the pressure condition of -0.98 MPa. After the reaction, the organotin acetate (DSDA) can be weighed and detected to reach the initial input amount, and then returned to the system for esterification. The yield of the sucrose-6 ester obtained after the reaction of the method is 88-92%, which is basically the same as the yield of the sucrose-6 ester obtained by the esterification and acylation operation with conventional newly added organotin.

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Abstract

The invention relates to a method for continuously preparing and supplementing an organic tin catalyst in sucralose production. The method comprises the following steps of pumping a cyclohexane phasecontaining organic tin acetate recovered after acylation in the previous batch into a distillation kettle, and supplementing 1-5% of dibutyltin oxide according to the amount of the organic tin acetateadded before esterification, and heating to a certain temperature, keeping the temperature, performing reacting, distilling under reduced pressure to remove the solvent after the reaction, and reusing the prepared organic tin acetate in the sucralose production process. According to the method, the acylation reaction of the dibutyltin oxide is carried out by fully utilizing the acetic anhydride remained in the cyclohexane extraction phase recovered in the previous batch in the production, so that the production device and the production cost of the sucralose catalyst are saved, the process issimplified, the production efficiency is greatly improved, the working intensity of operators is reduced, the pollution is reduced, and the environment is protected. The utilization rate of residualraw material is increased by using a novel process, so that the reaction efficiency and the material utilization rate are optimized in the whole production process, and the economic benefit of an enterprise is obviously increased.

Description

technical field [0001] The invention relates to a technical transformation of the production of sucralose, in particular to a supplementary method for the continuous preparation of an organotin catalyst in the production of sucralose. 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 organotin acetate (DSDA) in the more general sucralose production process mainly goes through the following process: dibutyltin oxide solid is dispersed in a solvent, and then acetic anhydride is added dropwise to rais...

Claims

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Application Information

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IPC IPC(8): C07H5/02C07H1/00C07H13/06
CPCC07H5/02C07H1/00C07H13/06
Inventor 张正颂沈东东李广馨杨志健
Owner ANHUI JINGHE IND
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