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Single solvent reaction method for sucralose esterification

A technology of sucralose and esterification reaction kettle, which is applied in chemical instruments and methods, esterification saccharides, organic chemistry, etc., can solve the problems of high energy consumption for solvent recovery, shortened production cycle, complicated process, etc., and achieve cost saving Consumption, shorten the production cycle, reduce the effect of raw material and energy consumption

Active Publication Date: 2019-02-26
ANHUI JINHE IND CO LTD
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Problems solved by technology

[0003] The purpose of the present invention is to solve the defects of complex process, high energy consumption of solvent recovery, and large pollution in the prior art, to provide a single-solvent reaction method for sucralose esterification, shorten the production cycle, save the original organic tin recovery treatment, Reduce the consumption of raw materials and energy and greatly improve the yield of products

Method used

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  • Single solvent reaction method for sucralose esterification
  • Single solvent reaction method for sucralose esterification
  • Single solvent reaction method for sucralose esterification

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Embodiment Construction

[0014] like figure 2 As shown, accurately put 700L of DMF and 1200L of DMF recovered from the previous batch into the esterification kettle, and put 300kg of sucrose into the esterification kettle, heat up, control the steam pressure at 1.8-2.0mpa, and turn off when the temperature rises to 70℃ Steam valve, let it naturally heat up to 84 ~ 86 ℃ and stir for 1.5 hours to fully dissolve the sugar.

[0015] Turn on the vacuum pump and control the vacuum negative pressure at -0.085~-0.09mpa, pour 600kg of organotin acetate into the esterification kettle, and turn on the steam to raise the pressure at 0.04~0.05MPa to control the temperature of the kettle At 68~70℃, under the condition of negative pressure -0.098mpa~-0.01mpa, the temperature of the kettle is normally at 76~78℃, continue to bring the negative pressure to cool down until the temperature of the kettle drops to 68~70℃ (observe the distillation situation during the test) ), open the steam valve, and control the steam p...

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Abstract

The invention relates to a method for the reaction of sucralose esterified single solvent, characterized by: 1) DMF, sucrose and organotin acetate are subjected to negative pressure esterification in an esterification kettle while DMF is recovered to the bypass channels of earlier stage by negative pressure distillation and condensing, and the recovered DMF whose water content is larger than 0.9-1.0% ppm is to be delivered into the recovery system; 2) Negative pressure recovery of DMF continues until the water content is less than 0.6% ppm, then which is returned to the esterification kettle for the next batch of esterification reaction; 3) The esterification reaction material is added into the esterification kettle, and acetic anhydride is added dropwisely in; water is added after adding dropwisely, and sucrose 6 ester and organotin acetate are extracted and separated with cyclohexane; organic tin acetate present in the cyclohexane phase, which is produced through evaporating of the cyclohexane solvent. The advantages of the method for the reaction of sucralose esterified single solvent is shortening the production cycle, eliminating the original tin recovery process, reducing the consumption of raw materials and energy and maximizing the savings in all costs.

Description

Technical field [0001] The invention relates to the field of food additive production, specifically a single-solvent reaction method for sucralose esterification. Background technique [0002] like figure 1 As shown, in the existing sucralose production, as the first step of the esterification reaction, DMF and cyclohexane are used as solvents and the traditional dehydration reaction method of adding catalyst organotin is used. After the reaction is completed, cyclohexane is used for extraction. The organotin acetate in the reaction solution is then distilled under normal pressure to recover cyclohexane. The remaining slurry organotin acetate is dissolved in methanol and then added dropwise to the sodium hydroxide solution for neutralization. After neutralization, the organotin is Produced in solid form, filtered and washed for reuse, this will produce a large amount of washing wastewater and a certain amount of steam and solvent will be consumed to recover DMF, cyclohexane...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/00C07H5/02C07F7/22
CPCC07H1/00C07H5/02C07H13/06
Inventor 赵金刚徐杰
Owner ANHUI JINHE IND CO LTD
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