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Preparation method of acesulfame potassium composition

A technology of acesulfame potassium and acesulfame acid, which is applied in the field of preparation of acesulfame potassium composition, can solve problems such as affecting product quality, and achieve the effects of improving product quality and reducing organic impurity content

Pending Publication Date: 2021-10-29
NANTONG ACETIC ACID CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Conventional methods improve the yield of the ring-closure reaction by changing the feed ratio of the ring-closure reaction, residence time, reaction temperature, and reactor structure, but there are few methods from the pH of the raw material acesulfame base triethylamine salt solution of the ring-closure reaction From the perspective of value, investigate its influence on the yield of the cyclization reaction, and then affect the quality of the product

Method used

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  • Preparation method of acesulfame potassium composition
  • Preparation method of acesulfame potassium composition
  • Preparation method of acesulfame potassium composition

Examples

Experimental program
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Effect test

Embodiment 1

[0078] 97g sulfamic acid is added in 700g dichloromethane solvent, then add 105g triethylamine to it and carry out neutralization reaction; Add 5.8g acetic acid in the synthetic resultant of sulfamic acid and triethylamine, neutralize redundant triethylamine , and control the pH value of the neutralization reaction solution to 6.5; add 85g of diketene to the neutralization reaction solution for acylation reaction, and obtain 992.8g of acetoacetamide-N-sulfonate. The acetoacetamide-N-sulfonate undergoes cyclization reaction with sulfur trioxide solution, and then undergoes hydrolysis reaction with water, and the cyclization hydrolysis yield is over 95.2%. The hydrolyzed acid layer was extracted with dichloromethane, and the dichloromethane layer was back-extracted with water. The dichloromethane layer after stripping is neutralized and layered with the prepared 7%-10% potassium hydroxide solution, and the neutralized water layer is concentrated, refined and dried to obtain refi...

Embodiment 2

[0080] 97g sulfamic acid is added in the 700g dichloromethane solvent, then add 105g triethylamine to it and carry out neutralization reaction; Add 8.1g propionic acid in the synthetic resultant of sulfamic acid and triethylamine, neutralize excess triethylamine amine, and control the pH value of the neutralization reaction solution to 5.5; add 85g of diketene to the neutralization reaction solution for acylation reaction, and obtain 905.1g of acetoacetamide-N-sulfonate. The acetoacetamide-N-sulfonate undergoes cyclization reaction with sulfur trioxide solution, and then undergoes hydrolysis reaction with water, and the cyclization hydrolysis yield is over 95%. The hydrolyzed acid layer was extracted with dichloromethane, and the dichloromethane layer was back-extracted with water. The dichloromethane layer after stripping is neutralized and layered with the prepared 7%-10% potassium hydroxide solution, and the neutralized water layer is concentrated, refined and dried to obta...

Embodiment 3

[0082] 58.2g sulfamic acid is joined in the 500g dichloromethane solvent, then adds 66.3g triethylamine to it and carries out neutralization reaction; Triethylamine, and control the pH value of the neutralization reaction solution to 6; add 52.1g of diketene to the neutralization reaction solution for acylation reaction to obtain 681g of acetoacetamide-N-sulfonate. The acetoacetamide-N-sulfonate undergoes cyclization reaction with sulfur trioxide solution, and then undergoes hydrolysis reaction with water, and the cyclization hydrolysis yield is over 95.3%. The hydrolyzed acid layer was extracted with dichloromethane, and the dichloromethane layer was back-extracted with water. The dichloromethane layer after stripping is neutralized and layered with the prepared 7%-10% potassium hydroxide solution, and the neutralized water layer is concentrated, refined and dried to obtain refined acesulfame potassium Composition with a chroma value of 0.3 Hazen. The acesulfame potassium c...

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Abstract

The invention relates to a preparation method of an acesulfame potassium composition. According to the preparation method, a proper amount of organic acid is added to adjust the pH value of a neutralization reaction solution so as to change the pH value of an acetoacesulfame triethylamine salt solution generated by acylation reaction, so that the subsequent cyclization hydrolysis yield is increased to 95% or above, and therefore, the content of organic impurities in the acesulfame potassium composition finished product is reduced, and the product quality is improved.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of an acesulfame potassium composition. Background technique [0002] Acesulfame potassium, the chemical name is 6-methyl-1,2,3-oxathiazin-4(3)-one-2,2-potassium dioxide, commonly known as acesulfame potassium, AK sugar (Acesulfame-K) . Because acesulfame potassium has the advantages of safety, non-toxicity, stable property, refreshing sweet taste, no bad aftertaste, and reasonable price, it is one of the most stable sweeteners in the world at present. It is used in food, medicine, etc. sweetener. [0003] In a conventional acesulfame potassium production process, sulfamic acid is reacted with an amine (eg, triethylamine) to form an ammonium sulfamate. The ammonium sulfamate solution is then reacted with diketene to form acesulfame triethylamine salt solution. Acesulfame potassium is cyclized, hydrolyzed and neutralized to form acesulfame potass...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D291/06
CPCC07D291/06
Inventor 俞新南庆九朱小刚刘芳
Owner NANTONG ACETIC ACID CHEM
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