Preparation method of acetoacetamide-N-sulfonic acid triethylamine salt

A technology of triethylamine sulfonate and acetoacetamide, which is applied in the field of preparation of acetoacetamide-N-triethylamine sulfonate, can solve the problems of unsatisfactory large-scale continuous production, slow reaction speed, long reaction time, etc. problems, to achieve the effect of simplifying the product post-processing process, good product appearance, and reducing production costs

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

However, there are still problems of slow reaction speed, long reaction time, and low yield, which cannot m...

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  • Preparation method of acetoacetamide-N-sulfonic acid triethylamine salt
  • Preparation method of acetoacetamide-N-sulfonic acid triethylamine salt

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preparation example Construction

[0023] The preparation method of acetoacetamide-N-sulfonic acid triethylamine salt of the present application comprises:

[0024] Amination reaction steps: dissolving sulfamic acid in the first dichloromethane to configure the first reaction solution; dissolving triethylamine in the second dichloromethane to configure the second reaction solution, adding the second reaction solution to Amination reaction is carried out in the first reaction solution to form ammonium sulfamate solution.

[0025] At first, be the preparation of sulfamic acid ammonium salt, specifically, sulfamic acid and triethylamine are dissolved in methylene chloride respectively, sulfamic acid and triethylamine exothermic reaction, in the reaction process, the heat that produces will Part of the dichloromethane is vaporized, and the vaporized dichloromethane will leave the reaction system to take away the heat produced. Further, the vaporized dichloromethane can also be recycled.

[0026] The first reaction...

Embodiment 1

[0059] Embodiment 1 (comprising embodiment 1A, embodiment 1B, embodiment 1C, implementing comparative example 1D, implementing comparative example 1E)

[0060] Amination reaction steps: Dissolve 98kg of sulfamic acid and the first dichloromethane at a molar ratio of 1:6, and control the dissolution temperature at about 20-25°C to obtain the dichloromethane solution of sulfamic acid as the first reaction solution. Dissolution can be in a continuous mixing device or in a reactor. Dissolving triethylamine and dichloromethane in a molar ratio of 1:1, controlling the dissolution temperature to be 10-30°C, to obtain a second reaction solution, wherein the mass ratio of sulfamic acid to triethylamine is 1: 1-1.2. Gradually drop the second reaction liquid into the reaction kettle where the first reaction liquid is located for mixing and stirring, and control the system to be weakly alkaline. After mixing evenly, the ammonium sulfamate solution is obtained.

[0061] Embodiment 1A,...

Embodiment 2

[0067] Embodiment 2 (comprising embodiment 2A, embodiment 2B, embodiment 2C, implementing comparative example 2D, implementing comparative example 2E)

[0068] Amination reaction steps: Dissolve 98kg of sulfamic acid and the first dichloromethane at a molar ratio of 1:15, and control the dissolution temperature at about 20-25°C to obtain the dichloromethane solution of sulfamic acid as the first reaction solution. Dissolution can be in a continuous mixing device or in a reactor. Dissolving triethylamine and dichloromethane in a molar ratio of 1:1.2, controlling the dissolution temperature to be 10-30°C, to obtain a second reaction solution, wherein the mass ratio of sulfamic acid to triethylamine is 1: 1-1.2. Gradually drop the second reaction liquid into the reaction kettle where the first reaction liquid is located for mixing and stirring, and control the system to be weakly alkaline. After mixing evenly, the ammonium sulfamate solution is obtained.

[0069] Embodiment ...

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Abstract

The invention provides a preparation method of acetoacetamide-N-sulfonic acid triethylamine salt, which comprises the following steps: dissolving sulfamic acid in first dichloromethane to prepare a first reaction solution; dissolving triethylamine in second dichloromethane to prepare a second reaction solution, and adding the second reaction solution into the first reaction solution for amination reaction to form an ammonium sulfamate solution; filling a zeolite catalyst into a fixed bed reactor, sequentially introducing the ammonium sulfamate solution and diketene into the fixed bed reactor, and reacting under preset conditions to form the acetoacetamide-N-triethylamine sulfonate solution. On one hand, the post-treatment process of the product is simplified, so that the final product acesulfame is better in appearance, and the use feeling is remarkably improved; on the other hand, large-scale continuous production of the acetoacetamide-N-sulfonic acid triethylamine salt is realized, the reaction time is greatly shortened, the reaction yield is improved, and the production cost of acesulfame potassium is further reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of acetoacetamide-N-sulfonic acid triethylamine salt. 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] Acetoacetamide-N-sulfonic acid triethylamine salt is the important intermediate of producing acesulfame potassium, and the preparation method of this intermediate generally adopts diketene-sulfur trioxide me...

Claims

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Application Information

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IPC IPC(8): C07C209/00C07C211/05C07C303/34C07C307/02B01J29/40
CPCC07C209/00C07C211/05C07C303/34C07C307/02B01J29/40Y02P20/584
Inventor 周睿丁震陈永旭杨峰宝刘刚
Owner ANHUI JINGHE IND
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