Method for recovering organic tin acetate from waste floccules in sucralose production

A technology of sucralose and floc, which is applied in the field of recycling organotin acetate, can solve the problems of high energy consumption, poor catalytic efficiency, and low purity of DSDA recovery, and achieve good effect, stable production efficiency, and alkali hydrolysis effect Good results

Pending Publication Date: 2021-11-30
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 solve the problem of low recovery purity of DSDA, high energy consumption and poor catalytic efficiency in the process of esterification in the method for recovering organotin acetate (DSDA) in the patent publication number CN109651428A , providing a method for recovering organotin acetate (DSDA) from waste flocs in sucralose production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] a. Add 1,000ml of the waste floc aqueous solution obtained by layering treatment after the esterification reaction into a single-necked flask for heating and vacuum distillation, control the temperature at 100°C, and the distillation pressure at -0.09MPa, and distill off water and cyclohexane, etc. Volatile impurities were obtained to obtain 238g of black tar;

[0018] b. Weigh 200g of the dark brown tarry substance obtained in step a and mix it with 200ml of methanol to dissolve, and the dissolution temperature is normal temperature (25°C);

[0019] c. Configure 500ml of sodium hydroxide solution with a concentration of 5%, raise the temperature to 80°C, slowly add the mixed dark brown floc into the NaOH solution, and control the neutralization temperature at about 80°C. Stir for 2 hours, filter with a Buchner funnel, and wash with hot water until the washing water is colorless, dry the obtained dibutyltin oxide in an oven at 60°C for 12 hours, and obtain white dibutyl...

Embodiment 2

[0024] a. Add 1,000ml of the waste floc aqueous solution obtained by layering treatment after the esterification reaction into a single-necked flask for heating and vacuum distillation. The temperature is controlled at 90°C, and the distillation pressure is -0.09MPa. Water and cyclohexane, etc. are distilled off. Volatile impurities were obtained to obtain 226g of black tar;

[0025] b. Weigh 200g of the dark brown tarry substance obtained in step a and mix it with 300ml of ethanol to dissolve, and the dissolution temperature is normal temperature (25°C);

[0026] c. Configure 500ml of sodium hydroxide solution with a concentration of 5%, raise the temperature to 80°C, slowly add the mixed dark brown floc into the NaOH solution, and control the neutralization temperature at about 80°C. Stir for 2 hours, filter with a Buchner funnel, and wash with hot water until the washing water is colorless, dry the obtained dibutyltin oxide in an oven at 80°C for 5 hours, and obtain white d...

Embodiment 3

[0031] a. Add 1,000ml of the waste floc aqueous solution obtained by layering treatment after the esterification reaction into a single-necked flask for heating and vacuum distillation. The temperature is controlled at 95°C, the distillation pressure is -0.09MPa, and water and cyclohexane are removed by distillation. Volatile impurities were obtained to obtain 229g of black tar;

[0032] b. Weigh 200g of the dark brown tarry substance obtained in step a and mix it with 500ml of acetone to dissolve, and the dissolution temperature is normal temperature (25°C);

[0033] c. Configure 500ml of sodium hydroxide solution with a concentration of 5%, raise the temperature to 85°C, slowly add the mixed dark brown floc into the NaOH solution, and control the neutralization temperature at about 85°C. Stir for 2 hours, filter with a Buchner funnel, and wash with hot water until the washing water is colorless, dry the obtained dibutyltin oxide in an oven at 85°C for 6 hours, and obtain whi...

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PUM

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Abstract

The invention relates to a method for recovering organic tin acetate from waste floccules in sucralose production, which comprises the steps of distillation, neutralization, centrifugation, water separation, acylation and extraction, and is characterized in that between the distillation step and the neutralization step, a black brown floccule obtained by distillation is mixed with and dissolved in a protonic solvent according to a volume ratio of 10: (1-5); and crude dibutyltin oxide obtained through centrifugation in the neutralization step is dried at 40-100 DEG C to obtain dried crude dibutyltin oxide. The method has the advantages that the black brown floccule is dissolved with the protic solvent, the dispersion effect of the dibutyltin oxide in water can be promoted, the treated dibutyltin oxide powder is uniform in particle, the appearance of the product is similar to that of a pure product in color, the impurity content is low, and the production efficiency can reach the standard of a normal catalyst and is relatively stable; and the method is easy to operate, the reaction efficiency and the material utilization rate of the whole production process are optimized, and the economic benefits of enterprises are obviously increased.

Description

technical field [0001] The invention belongs to the technical field of food additive production, and in particular relates to a method for recovering organotin acetate from waste flocs in 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, after the reaction is completed, it is extracted by adding the extractant cyclohexane to form a DMF (N,N-dimethylamide, water and sucrose-6-acetate) layer and an extraction layer, and organotin acetate ( DSDA) is dissolved in the cyclohexane phase of the extrac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22B01J31/12C07H13/04C07H1/00
CPCC07F7/2224C07F7/2296B01J31/122C07H13/04C07H1/00B01J2231/49
Inventor 沈东东仇鑫慈昊
Owner ANHUI JINGHE IND
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