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Preparation method of acesulfame potassium

A technology of acesulfame potassium and acetoacetamide is applied in the field of preparation of acesulfame potassium, and can solve the problems of affecting the use experience, difficult separation of impurities, deep impurities, etc., to suppress the generation of by-products, reduce the production cost, and improve the Yield effect

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

[0004] In the prior art, on the one hand, acetic acid is usually added as a catalyst during the reaction process, which makes acetic acid impurities remain in the final product acesulfame potassium, resulting in poor color quality of acesulfame potassium and affecting people’s use experience
[0005] On the other hand, in the step of cyclization reaction between acetylacetamide salt and sulfur trioxide to form cyclic sulfur trioxide adduct, many impurities similar to the final product acesulfame potassium structure will be introduced, such as 5-chloro- Acesulfame potassium, etc. These impurities are difficult to separate in subsequent processing, and the impurities have a darker color, resulting in a light brown finished product of acesulfame potassium, which affects the quality of acesulfame potassium

Method used

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  • Preparation method of acesulfame potassium

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[0027] The preparation method of acesulfame potassium provided by the application at least includes step S110 to step S140:

[0028] Pretreatment step S110: treating the acetoacetamide-N-sulfonic acid triethylamine salt solution with a weakly basic inorganic substance to obtain an intermediate solution;

[0029] Acetoacetamide-N-sulfonic acid triethylamine salt is an intermediate for preparing acesulfame potassium, which can be prepared by any one or combination of several in the prior art. It is a mixture solution, in which at least There is residual acidic catalyst, usually acetic acid.

[0030] In the pretreatment step, the intermediate acetoacetamide-N-sulfonic acid triethylamine salt solution for preparing acesulfame potassium is pretreated by using weakly basic inorganic substances. On the one hand, weakly basic inorganic substances can remove residual acidic catalysts , on the other hand, it can provide a slightly alkaline reaction environment for the cyclization react...

Embodiment 1( Embodiment 1A

[0079] Example 1 (Example 1A, Example 1B, Example 1C, Example 1D, Example 1E, Example 1F)

[0080] Pretreatment step: treating the acetoacetamide-N-sulfonic acid triethylamine salt solution with potassium carbonate in different ratios to obtain an intermediate solution.

[0081] Sulfonation and cyclization step: dissolving sulfur trioxide in a solvent to form a cyclizing agent solution; performing a sulfonation and cyclization reaction between the intermediate solution and the cyclizing agent solution to obtain a sulfonation and cyclization product;

[0082] Hydrolysis step: adding a hydrolyzing agent to the sulfonated cyclization product solution to carry out a hydrolysis reaction to obtain a hydrolyzate solution; and

[0083] Salt-forming step: adding an ethanol solution of potassium hydroxide to the organic phase of the hydrolyzate solution to carry out a salt-forming reaction to obtain acesulfame potassium. In each embodiment, only the molar ratio of potassium carbonate a...

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Abstract

The invention discloses a preparation method of acesulfame potassium, which comprises the following steps: a pretreatment step: treating an acetoacetamide-N-sulfonic acid triethylamine salt solution by using a weakly alkaline inorganic substance to obtain an intermediate solution; a sulfonation cyclization step: dissolving sulfur trioxide in a solvent to form a cyclizing agent solution, and carrying out sulfonation cyclization reaction on the intermediate solution and a cyclizing agent solution to obtain a sulfonation cyclization product; a hydrolysis step: adding a hydrolysis agent into the sulfonation cyclization product solution, and carrying out a hydrolysis reaction to obtain a hydrolysis product solution; and a salt-forming step: adding a salt-forming agent into the organic phase of the hydrolysate solution, and carrying out a salt-forming reaction to obtain acesulfame potassium. On the one hand, the acid catalyst remaining in the final product acesulfame potassium is removed; on the other hand, the reaction environment provided by the alkalescent inorganic matter inhibits the generation of by-products and provides the purity of the acesulfame potassium product; the yield of the acesulfame potassium can be remarkably improved, 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): C07D291/06
CPCC07D291/06
Inventor 周睿丁震陈永旭杨峰宝刘刚
Owner ANHUI JINGHE IND
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