Continuous acylation synthesis method in acesulfame potassium synthesis

A technology for the synthesis of acesulfame potassium, which is applied in the chemical industry, can solve problems such as difficult stability of product quality, and achieve the effects of solving unstable quality and potential safety hazards, low overall cost, and reducing labor intensity and equipment investment

Active Publication Date: 2020-12-29
NANTONG ACETIC ACID CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, this method adopts the batch reaction mode, which has disadvantages such as the need for loading and unloading, cleaning and other auxiliary processes, and the product quality is not easy to stabilize.

Method used

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  • Continuous acylation synthesis method in acesulfame potassium synthesis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 600g of neutralization reaction solution (containing 0.76mol of sulfamic acid) into the acylation kettle 1, then start stirring, and slowly add 78.2g of diketene ketone dropwise. During the process, the reaction temperature is controlled at 20-25°C, and the dropwise addition time is 40min. After the addition of diketene ketone is completed Finally, keep warm at 20-25°C for 1.5h to complete the preparation of the bottoming solution.

[0042] The neutralization reaction solution 30g / h and diketene 3.9g / h are continuously fed into the acylation kettle 1; the residence time of each acylation kettle is 1h, and it overflows to the acylation kettle 2 by means of overflow, and the acylation kettle 2 passes through The overflow method overflows to the acylation kettle 3, and the acylation kettle 3 overflows to the acylation kettle 4 by means of overflow, and the residence time is 4 hours in total. During the process, the temperature of each acylation kettle is controlled at 2...

Embodiment 2

[0044] Add 600g of neutralization reaction solution (containing 0.76mol of sulfamic acid) into the acylation kettle 1, then start stirring, and slowly add 71.66g of diketene ketone dropwise. During the process, the reaction temperature is controlled at 25-30°C, and the dropwise addition time is 20min. The addition of diketene ketone is completed. Finally, keep warm at 20-25°C for 1 hour to complete the preparation of the bottoming solution.

[0045]The neutralization reaction solution 30g / h and diketene 3.5g / h are continuously fed into the acylation kettle 1; the residence time of each acylation kettle is 1h, and it overflows to the acylation kettle 2 by means of overflow, and the acylation kettle 2 passes through The way of overflow overflows to the acylation kettle 3, and the residence time is 3 hours in total. During the process, the temperature of each acylation kettle is controlled at 25-35°C, and the acylation kettle 3 overflows to the receiving kettle by overflowing, and...

Embodiment 3

[0047] Add 600g of neutralization reaction solution (containing 0.76mol of sulfamic acid) into the acylation kettle 1, then start stirring, and slowly add 65.2g of diketene ketone dropwise. During the process, the reaction temperature is controlled at 25-30°C, and the dropwise addition time is 20min. The addition of diketene ketone is complete Finally, keep warm at 20-25°C for 1 hour to complete the preparation of the bottoming solution.

[0048] 30g / h of the neutralization reaction solution and 2.5g / h of diketene are continuously fed into the acylation kettle 1; the residence time of each acylation kettle is 1h, and it overflows to the acylation kettle 2 by means of overflow, and the acylation kettle 2 passes through The way of overflow overflows to the acylation kettle 3, and the residence time is 3 hours in total. During the process, the temperature of each acylation kettle is controlled at 25-35°C, and the acylation kettle 3 overflows to the receiving kettle by overflowing,...

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Abstract

The invention belongs to the field of chemical production, and particularly relates to a continuous acylation synthesis method in acesulfame potassium synthesis, wherein the method comprises the following steps: partially paving a synthesis material of sulfamic acid and triethylamine, namely a neutralization reaction solution, dropwisely adding a certain amount of diketene, reacting to obtain a preparation solution, continuously feeding the neutralization reaction solution and diketene into a reactor, and carrying out continuous acylation reaction to obtain a DKA reaction solution. Compared with traditional single-kettle intermittent dropwise adding of diketene, the method has the advantages that the heat exchange speed is increased, the production period is shortened, the production efficiency is improved, and meanwhile, the problems of unstable quality, potential safety hazards and the like caused by manual operation are solved.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a continuous acylation synthesis method in the synthesis of acesulfame potassium. Background technique [0002] Acesulfame potassium (acesulfame potassium), 6-methyl-1,2,3-oxazin-4-(3H)-one-2,2-dioxide; 6-methyl-1,2, 3-oxazin-4-(3H)-one-2,2-dioxopotassium salt; 6-methyl-1,2,3-oxazin-4-(3H)-one-2,2- Dioxopotassium salt; 6-methyl-2,2-dioxo-1,2,3-oxathiazepine; acesulfame potassium; 6-methyl-1,2,3-oxazine-4- (3H)-keto-2,2-dioxy potassium salt; AK sugar English name: RARECHEM AM UC 0205; SWEET ONE; SUNETTE; POTASSIUM 6-METHYL-1,2,3-OXATHIAZIN-4(3H)-ONE 2 ,2-DIOXIDE; 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide; acesulfame; ACESULFAME K; ACESULFAME POTASSIUM. Appearance properties: white crystalline powder, easily soluble in water, slightly soluble in ethanol; CAS number: 55589-62-3; [0003] Molecular formula: C4H4KNO4S; molecular weight: 201.2; melting poi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D291/06
CPCC07D291/06
Inventor 庆九俞新南薛金全朱小刚刘芳
Owner NANTONG ACETIC ACID CHEM
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