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Recovery method of organotin in sucralose production

A technology of sucralose and recovery method, which is applied in the direction of sugar derivatives, chemical recovery, sugar derivatives, etc., can solve the problems of complicated steps and large amount of sewage, and achieve the improvement of production efficiency, product quality and material utilization rate optimized effect

Active Publication Date: 2017-11-17
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the shortcomings of complex steps and large amount of sewage generated in the existing organotin recovery method, and provide a method for recovering organotin in the production of sucralose

Method used

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Examples

Experimental program
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Effect test

Embodiment Construction

[0014] 1. Collect the cyclohexane phase containing organotin acetate after extraction and stratification and put it into the cyclohexane phase tank;

[0015] 2. Pump about 5000L of the cyclohexane phase extracted in batches into the cyclohexane phase washing kettle, add 600L of pure water, start stirring, the temperature is 35°C, the stirring time is 2 hours, and then stand still for 1 hour;

[0016] 3. Then separate the layers, separate the water phase at the bottom of the washing tank to the water phase tank, and separate the cyclohexane phase to the cyclohexane phase tank;

[0017] 4. Pump 5000L of the cyclohexane phase into the cyclohexane recovery kettle, start the steam to recover cyclohexane under reduced pressure;

[0018] 5. When the temperature of the recovery kettle rises to 100°C or little cyclohexane is evaporated (discharged in a linear form), the recovery reaction ends;

[0019] 6. Close the steam valve, turn on the cooling water to cool down the material in th...

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Abstract

The invention relates to a recovery method of organotin in the production of sucralose, which comprises the esterification reaction of sucralose, in which dibutyltin oxide is used as a catalyst to participate in the reaction to generate a sucrose hexaester intermediate, and after the intermediate solution is extracted by cyclohexane, the organotin Acetate is dissolved in the cyclohexane phase of the extraction agent, the cyclohexane phase is separated, and the cyclohexane is evaporated by a distillation pot; it is characterized in that it includes the following steps: a. Open cooling water to cool to 50 ° C, and then add pure Stir and wash with water for 1 hour; b. Separate the bottom water, and the residue in the kettle is recovered organotin acetate, return to the esterification kettle to participate in the esterification reaction and reuse it. Advantages of the invention: organotin acetate does not undergo degreasing and drying, and is recycled and reused directly, so as to achieve zero discharge, reduce production costs, solve waste water generated in the process of organotin recovery to the greatest extent, and greatly improve production efficiency , significant economic benefits.

Description

Technical field: [0001] The invention relates to a method for recovering organotin dibutyltin oxide in the production of sucralose. Background technique: [0002] The recovery of organotin in the traditional sucralose production process mainly goes through the following process: the organotin dissolved in the solution after the esterification exists in the form of organotin acetate, and is extracted by adding the extractant cyclohexane to form DMF (N , N-dimethylamide, water and sucrose-6 ester) layer and extraction layer, organotin acetate is dissolved in the cyclohexane phase of the extraction layer, and then the cyclohexane phase is separated and placed in a still After recovering the extraction agent cyclohexane through steam heating, it is dissolved in methanol and pumped into the high-position dripping tank, and added dropwise to the organotin recovery kettle with sodium hydroxide solution in advance, and then the steam is heated to evaporate and recover methanol, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/00C07H13/06
CPCY02P20/584
Inventor 张正颂
Owner ANHUI JINGHE IND
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