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Preparation method of acesulfame potassium

A technology of acesulfame potassium and sulfamic acid, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problem of low yield of finished products of acesulfame potassium, easy decomposition of cyclization products, and hydrolysis reactions Low yield and other problems, to achieve the effect of improving acylation reaction efficiency, reducing production cost and increasing yield

Active Publication Date: 2021-09-28
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the reaction time is long, the cyclization product is easy to decompose, the yield of the hydrolysis reaction is low, and the finished product yield of acesulfame potassium is low, and the quality of the finished product is relatively poor

Method used

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preparation example Construction

[0031] The preparation method of acesulfame potassium provided by the application at least includes step S110 to step A140:

[0032] Intermediate preparation step S110: adding triethylamine to the sulfamic acid solution for amination reaction to generate a sulfamic acid ammonium salt solution; , carry out the acylation reaction to obtain the intermediate solution.

[0033] The preparation of the intermediate is more carefully divided into two small steps. First, it is the preparation of ammonium sulfamate, and then the intermediate is prepared by reacting ammonium sulfamate with diketene, that is, acetoacetamide-N-sulfonic acid triethyl amine salt.

[0034] The ammonium salt of sulfamic acid is obtained by adding triethylamine to the sulfamic acid solution for amination reaction. Specifically, in some embodiments of the present application, sulfamic acid is dissolved in the first solvent to configure the first reaction solution; triethylamine is dissolved in the second solve...

Embodiment 1

[0073] Example 1 (Example 1A, Example 1B, Example 1C, Example 1D, Example 1E, Example 1F, Example 1G, Example 1H)

[0074]Preparation of intermediate solution: When preparing intermediate solution, use super acid SO 4 2- / Fe 2 o 3 As a catalyst, other steps refer to the preparation of intermediate solution A.

[0075] Sulfonation and cyclization step: dissolving sulfur trioxide in dichloromethane to form a cyclization agent solution; adding the cyclization agent solution to the intermediate solution to carry out sulfonation and cyclization reaction to obtain a cyclization product solution.

[0076] Hydrolysis step: adding ethanol aqueous solution as a hydrolysis agent to the cyclization product solution to carry out hydrolysis reaction to obtain a hydrolyzate solution.

[0077] Salt-forming step: adding an ethanol solution of potassium hydroxide to the organic phase of the hydrolyzate solution to obtain acesulfame potassium. Please refer to Table 1 for specific reaction c...

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Abstract

The invention discloses a preparation method of acesulfame potassium, which comprises the following steps: adding triethylamine into a sulfamic acid solution, and carrying out amination reaction to generate an ammonium sulfamic acid salt solution; adding diketene into the obtained ammonium sulfamate solution, and carrying out acylation reaction under the action of a solid superacid catalyst to obtain an intermediate solution; dissolving sulfur trioxide in a solvent to form a cyclizing agent solution; adding a cyclizing agent solution into the intermediate solution, and carrying out sulfonation cyclization reaction to obtain a cyclization product solution; adding a hydrolytic agent into the cyclization product solution, and carrying out hydrolysis reaction to obtain a hydrolysate solution; and adding a potassium hydroxide solution into the organic phase of the hydrolysate solution to obtain acesulfame potassium. According to the method, the content of impurities in the acesulfame potassium can be reduced, so that the acesulfame potassium is better in condition, the conversion rate of the raw materials is increased, the yield of a cyclization product is increased to a great extent, further, the yield of the final product acesulfame potassium is increased, and the production cost of the acesulfame potassium is reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemical manufacturing, and in particular relates to a preparation method of acesulfame potassium. Background technique [0002] Acesulfame potassium (acesulfame potassium), also known as AK sugar, is a widely used sugar substitute food additive. Its appearance is white crystalline powder. As an organic synthetic salt, its taste is similar to sugarcane, and it is easily soluble in water. , Slightly soluble in alcohol, its chemical properties are stable, and it is not easy to break down and fail; it does not participate in the body's metabolism and does not provide energy; it has high sweetness and low price; it has no cariogenicity; it has good stability to heat and acid. [0003] At present, in the synthesis of acesulfame potassium, the diketene-sulfur trioxide method is widely used. The specific reaction steps include: reacting sulfamic acid with amine to form amine sulfamic acid salt, and then rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D291/06B01J27/053
CPCC07D291/06B01J27/053B01J23/745
Inventor 周睿丁震陈永旭杨峰宝刘刚
Owner ANHUI JINGHE IND
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