Method for high-temperature continuous acylation in sucralose production

A sucralose, medium and high temperature technology, applied in the chemical industry, can solve the problems of energy consumption, low reaction yield, low reaction temperature, etc., and achieve the effects of improving operating temperature, product purity, and high reaction yield

Inactive Publication Date: 2019-03-08
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The acylation reaction in the production process of sucralose is basically carried out at an acylation temperature of -2 to 2°C. It is carried out intermittently in the reactor, the reaction temperature is low, the reaction is slow, and the operation is intermittent, the reaction conditions are not easy to control, and the yield is low.
Moreover, the reaction temperature is controlled at -2~2°C, which needs to be cooled by -15°C frozen brine to ens

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  • Method for high-temperature continuous acylation in sucralose production

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Example Embodiment

[0013] Example 1

[0014] Pump the esterification liquid containing sucrose organotin intermediate (including intermediate: 65wt%, DMF: 35wt%) and acetic anhydride into the acylation reactor at the same time, the temperature of the reactor is about 30℃, the esterification liquid and acetic anhydride The mass ratio is 10:1, while adjusting the flow rate of acetic anhydride to make the pH value of the mixture after the reaction reach 4.5, the acylation reaction can be completed in 0.2s. The material at the outlet of the acylation reactor enters the acylation freezer to cool down at 10-15°C, keep it warm with chilled water, and keep it for 1 hour.

[0015] The acylation reaction solution is then subjected to a hydrolysis reaction, and then cyclohexane is added for extraction to recover the organotin acetate produced after the reaction. The content of sucrose-6-ethyl ester in the acylation reaction solution is detected, and the reaction yield is ≥98%.

[0016] The organotin acetate extr...

Example Embodiment

[0017] Example 2

[0018] The esterification liquid containing sucrose organotin intermediate: intermediate: 65wt%, DMF: 35wt% esterified liquid is pumped into the acylation reactor, and acetic anhydride is pumped to adjust the flow rate to make the pH value of the mixture after the reaction to 5, esterification The liquid and acetic anhydride are pumped into the acylation reactor at the same time, the mass ratio of esterification liquid to acetic anhydride is 13:1, the temperature of the reactor is controlled at 10-15℃, and the reaction time is controlled at 0.2s. The material at the outlet of the reactor enters the acylation. In the freezing kettle, use circulating water for heat preservation.

[0019] The acylation reaction solution is then subjected to a hydrolysis reaction, and then cyclohexane is added for extraction to recover the organotin acetate produced after the reaction. The content of sucrose-6-ethyl ester in the acylation reaction solution is detected, and the reacti...

Example Embodiment

[0021] Example 3

[0022] The esterification liquid containing sucrose organotin intermediate: intermediate: 65wt%, DMF: 35wt% esterified liquid is pumped into the acylation reactor, and acetic anhydride is pumped to adjust the flow rate to make the pH value of the mixture after the reaction to 5, esterification The liquid and acetic anhydride are pumped into the acylation reactor at the same time, the mass ratio of esterification liquid to acetic anhydride is 15:1, the temperature of the reactor is controlled at 10-15℃, and the reaction time is controlled at 0.2s. The material at the outlet of the reactor enters the acylation. In the freezing kettle, use circulating water for heat preservation.

[0023] The acylation reaction solution is then subjected to a hydrolysis reaction, and then cyclohexane is added for extraction to recover the organotin acetate produced after the reaction. The content of sucrose-6-ethyl ester in the acylation reaction solution is detected, and the reacti...

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Abstract

The invention relates to a method for high-temperature continuous acylation in sucralose production. The method comprises the following steps: a, conveying esterification liquid obtained from an esterification reaction to an inlet of an acylation reactor by a pump; b, conveying acetic anhydride to a side inlet of the acylation reactor by a pump, performing an acylation reaction on the esterification liquid and the acetic anhydride in the acylation reactor, wherein the temperature of the reactor is between 25 and 35 DEG C, the mass flow ratio of the esterification liquid to the acetic anhydrideis 10:1 to 15:1, and the pH value after the acylation reaction is 4.5-5.5; and c, conveying a mixed solution after the acylation reaction to an acylation kettle for cooling, and controlling the temperature at 10-15 DEG C. The method provided by the invention has the advantages that an acylation reaction can be continuously realized by a reactor, and full-automatic control is adopted, so that theproduction efficiency is greatly improved, the reaction temperature is increased, the production energy consumption is greatly reduced, the production cost is reduced, and the production reaction yield is improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a high-temperature continuous acylation method in the production of sucralose. Background technique [0002] Sucralose is a fresh sweetener, its sweetness is 600-800 times that of sucrose, and its sweetness is similar to that of sucrose. Sucralose is not absorbed by the human body, has no bioaccumulation, and has high safety. The sucrose industry developed rapidly, the number of production enterprises gradually increased, and the output continued to increase. The acylation reaction in the production process of sucralose is basically carried out at an acylation temperature of -2 to 2°C, and is carried out intermittently in a reactor, the reaction temperature is low, the reaction is slow, and the operation is intermittent, the reaction conditions are not easy to control, and the yield is low. Moreover, controlling the reaction temperature at -2 to 2°C require...

Claims

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Application Information

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IPC IPC(8): C07H13/04C07H1/00
CPCC07H1/00C07H13/04
Inventor 张正颂孙多龙易健康
Owner ANHUI JINGHE IND
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