Preparation method for sucralose

A technology of sucralose and sucrose, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the disadvantages of unfavorable automatic production and production cost control, sucralose-6-ethyl ester is easy to be thermally decomposed, Solve problems such as cumbersome process steps, achieve the effect of improving the level of clean production, improving the level of automated production, and shortening the process route

Active Publication Date: 2019-07-02
WENGYUAN GUANGYE QINGYI FOOD TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This treatment method has the defects of large energy consumption, cumbersome process steps, low product yield, and sucralose-6-ethyl ester is easy to be thermally decomposed, which is not conducive to automatic production and production cost control

Method used

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  • Preparation method for sucralose

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation method of sucralose provided in this example, further, the method of directly preparing sucralose from the extraction and separation intermediate (sucralose-6-ethyl ester aqueous solution), specifically includes the following steps:

[0031] (1) Take the reaction solution obtained by chlorination of sucrose-6-ethyl ester, add sodium hydroxide solution to adjust to pH = 9.0, then add concentrated hydrochloric acid to adjust to pH = 7.0, to obtain a neutralization solution;

[0032] (2) Filter the neutralization solution to remove salt, measure 500mL, 666.2g of the feed solution, add 250mL of clear water, extract 3 times, and combine the extraction phases; distill and remove DMF to obtain an extract containing sucralose-6-ethyl ester 335.32g, detected by high performance liquid chromatography, contains 8.23wt% of sucralose-6-ethyl ester, and 27.5968g of sucralose-6-ethyl ester can be obtained by calculation;

[0033] The raffinate phase recovers the inert ...

Embodiment 2

[0042] The preparation method of sucralose provided in this example, further, the method of directly preparing sucralose from the extraction and separation intermediate (sucralose-6-ester aqueous solution), specifically includes the following steps:

[0043] (1) adding sodium hydroxide solution to the reaction solution obtained by chlorination of sucrose-6-ethyl ester to adjust the pH to 9.0, and then adding concentrated hydrochloric acid to adjust the pH to 7.0 to obtain a neutralizing solution;

[0044] (2) Filter the neutralization liquid to remove salt, measure 500 mL of the feed liquid, 666.4 g as the first batch, add 250 mL of water in turn, and extract 3 times. The third extraction phase of the first batch was used for the first extraction of 500mL and 666.7g of the second batch of feed liquid, and then 250mL and 250mL of clear water were added in order to extract the second batch of feed liquid;

[0045]DMF was removed by distillation to obtain 320.25 g of the first ba...

Embodiment 3

[0049] The preparation method of sucralose provided in this example, further, the method of directly preparing sucralose from the extraction and separation intermediate (sucralose-6-ester aqueous solution), specifically includes the following steps:

[0050] (1) adding sodium hydroxide solution to the reaction solution obtained by chlorination of sucrose-6-ethyl ester to adjust the pH to 9.0, and then adding concentrated hydrochloric acid to adjust the pH to 7.0 to obtain a neutralizing solution;

[0051] (2) Filter the neutralization solution to desalt, measure 500mL, 666.2g of the feed solution, add 350mL, 150mL, 350mL of water in turn, extract 3 times, combine the extraction phases; distill to remove DMF, and obtain the sucralose-6- Ethyl ester extract 340.10g. After detection by high-performance liquid chromatography, it contains 7.54wt% of sucralose-6-ethyl ester, and 25.6485g of sucralose-6-ethyl ester can be obtained by calculation;

[0052] The raffinate phase recover...

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Abstract

The invention discloses a preparation method for sucralose. The method includes the following steps: performing neutralization treatment on a reaction liquid obtained by chlorinating sucrose-6-ethyl ester to obtain a neutralization solution, removing a salt from the neutralization solution and then adding an extraction agent, separating an extract phase including 4, 1', 6'-sucralose-6-ethyl esterand tertiary amide, removing a tertiary amide solvent in the extraction phase, then directly adding alkali for performing a deacylation reaction to obtain a sucralose crude product liquid, and then subjecting separation and purification to obtain a sucralose fine product. The method has the advantages of simple and short process, high yield, low production cost, and the like.

Description

technical field [0001] The invention belongs to the technical field of sucralose, relates to a preparation method of sucralose, in particular to a method for directly preparing sucralose by extracting and separating intermediates. Background technique [0002] Sucralose, a new chlorinated derivative of sucrose, is 600 times sweeter than sucrose. It has the characteristics of good taste, no caries, low calorific value and good thermal stability. It is currently the best high-intensity sweetener . [0003] The industrial production of sucralose mostly adopts the single-group protection method, and there are three main steps in the synthesis of sucralose by the single-group protection method: ①Esterification reaction: carry out ethyl esterification protection to the 6-position hydroxyl of sucrose, and obtain the esterified product (sucrose -6-ethyl ester); ②chlorination reaction: sucrose-6-ethyl ester uses a chlorinating agent (such as thionyl chloride, carbonyl chloride or tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H5/02
CPCC07H1/00C07H5/02Y02P20/55
Inventor 曾伟山张伟薇陈少华林杰卫娜
Owner WENGYUAN GUANGYE QINGYI FOOD TECH
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