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Preparation method of acesulfame potassium

A technology of acesulfame potassium and potassium ethoxide, applied in the direction of organic chemistry, etc., can solve the problems of low purity of acesulfame potassium, and it is difficult to further improve the product purity, and achieve the effect of improving the purity, reducing the content of inorganic impurities, and simplifying the process

Active Publication Date: 2021-09-28
ANHUI JINGHE IND
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Problems solved by technology

[0003] At present, in the synthesis of acesulfame potassium, the diketene-sulfur trioxide method is generally used, and the specific reaction steps include: reacting sulfamic acid with amine to form amino sulfonic acid amine salt, then react sulfamic acid amine salt with diketene to form acetyl acetamide salt; in the presence of sulfur trioxide, acetyl acetamide salt undergoes cyclization reaction to form cyclic sulfur trioxide adduct; The cyclic compound is hydrolyzed to obtain a hydrolyzate (ASH); then the hydrolyzate is usually treated with potassium hydroxide or potassium hydroxide aqueous solution to obtain acesulfame potassium (ASK), such as Chinese patent CN111228854A, Chinese patent CN1062560C and Chinese patent CN111377883A, etc., using Potassium hydroxide or potassium hydroxide aqueous solution carries out salt-forming reaction, and there are many problems, as in the process of separating, also there is a large amount of inorganic components in the product of direct precipitation, such as potassium fluoride, potassium sulfate etc., the product purity is difficult to further improve increase, causing the problem of low purity of the final product acesulfame potassium

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[0027] The preparation method of acesulfame potassium provided by the application at least includes step S110 to step S120:

[0028] Salt-forming step S110: separating the sulfonated cyclization product solution into an organic phase and an inorganic phase, adding an ethanol solution of potassium ethoxide to the organic phase to perform a salt-forming reaction; wherein, the sulfonated cyclization product solution is acetoacetamide-N- The cycloaddition product of triethylamine sulfonate and sulfur trioxide is obtained by hydrolysis.

[0029] In this application, the sulfonated cyclization product refers to the process of preparing acesulfame potassium by the diketene-sulfur trioxide method. In the presence of sulfur trioxide, the acetylacetamide salt undergoes a cyclization reaction to form a cyclic sulfur trioxide plus compound. compound, and then the hydrolysis product (ASH) obtained by hydrolysis of the cyclic compound is a sulfonated ring closure product.

[0030] In the p...

Embodiment 1( Embodiment 1A

[0076] Example 1 (Example 1A, Example 1B, Example 1C)

[0077] Salt-forming step: separating the above-mentioned sulfonated cyclization product solution into an organic phase and an inorganic phase, and adding a salt-forming reagent—a solution of potassium ethoxide in ethanol to the organic phase to carry out a salt-forming reaction. The specific reaction conditions are shown in Table 1.

[0078] Washing step: after the salt-forming reaction is completed, the solid product is obtained by filtration, and the solid product is washed with ethanol to obtain the crude product of acesulfame potassium.

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Abstract

The invention discloses a preparation method of acesulfame potassium, which comprises the following steps: a salt forming step: separating a sulfonation cyclization product solution into an organic phase and an inorganic phase, and adding an ethanol solution of potassium ethoxide into the organic phase for salt forming reaction, wherein the sulfonation cyclization product solution is obtained by hydrolyzing a product obtained by cyclization addition of acetoacetamide-N-sulfonic acid triethylamine salt and sulfur trioxide; and a washing step: after the salt forming reaction is finished, filtering to obtain a solid product, and washing the solid product with ethanol to obtain a crude acesulfame potassium product. According to the invention, the content of inorganic impurities in the acesulfame potassium crude product is greatly reduced, and the purity of the final product acesulfame potassium is remarkably improved; the subsequent process of the acesulfame potassium crude product is simplified, and the purification cost of the acesulfame potassium crude product is reduced; and the yield of acesulfame potassium can be improved.

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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IPC IPC(8): C07D291/06
CPCC07D291/06Y02P20/584
Inventor 周睿丁震陈永旭杨峰宝刘刚
Owner ANHUI JINGHE IND
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