Method for continuously producing acesulfame potassium
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A continuous, cyclizing agent technology, applied in the direction of organic chemistry, can solve the problem of difficult stability of product quality
Active Publication Date: 2020-07-07
NANTONG ACETIC ACID CHEM +1
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However, at present, this method adopts the batch reaction mode, which has disadvantages such as the need for l
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[0043] A method for continuous production of acesulfame K, comprising the steps of:
[0044] (1) Acylation section
[0045]1. Sulfamic acid and dichloromethane are continuously mixed and dissolved, and then continuously neutralized with triethylamine solution. The neutralization reaction solution and diketene enter the continuous reactor, and the DKA reaction solution is obtained through addition acylation reaction.
[0046] 2. The continuous mixing and dissolving, the molar ratio is: n (sulfamic acid): n (dichloromethane 1: 1 ~ 20, preferably 1: 8 ~ 12; the temperature is 0 ~ 40 ° C; preferably 15 ~ 25 ℃;
[0047] 3. The continuous neutralization, wherein neutralized pH=7~9; its triethylamine solution is a mixed solution of triethylamine and dichloromethane, and the molar ratio is n (triethylamine):n (dichloromethane) =1:0~5, preferably 1:0~2; neutralization temperature is 10°C~40°C, preferably 20°C~30°C.
[0048] 4. The addition acylation reaction, its molar ratio n(sulfa...
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Abstract
The invention belongs to the field of chemical production, and provides a method for continuously producing acesulfame potassium, which comprises the following steps: continuously mixing and dissolving sulfamic acid and dichloromethane, continuously neutralizing with a triethylamine solution, introducing the neutralized reaction solution and ketene dimer into a continuous reactor, and carrying outaddition acylation reaction to obtain a DKA reaction solution; sulfur trioxide and solvent micro-mixing: S03, enabling dichloromethane to enter a micro-mixer, so as to prepare a cyclizing agent; cyclization and hydrolysis: continuously feeding the DKA reaction solution and a cyclizing agent into a cyclization microreactor to generate a cyclization reaction solution, and continuously feeding the cyclization reaction solution into a hydrolysis microreactor to obtain an acesulfamic acid reaction solution; enabling the acesulfame acid reaction liquid and dichloromethane to enter continuous extraction equipment, enabling an extracted organic phase and a potassium hydroxide aqueous solution to enter a continuous neutralization reactor to obtain acesulfame acid potassium reaction liquid, and subjecting the acesulfame acid potassium reaction liquid to continuous concentration, continuous crystallization, continuous separation and continuous drying to obtain the acesulfame acid potassium finished product. The process has the characteristics of simple process, low cost, good product quality, continuous whole process and the like.
Description
technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for continuous production 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; ACE SULFAME K; Appearance properties: white crystalline powder, easily soluble in water, slightly soluble in ethanol; CAS number: 55589-62-3; molecular formula: C4H4KNO4S; molecular weight: 201.2; melting point: 225°; water solubility: 270g / L at 20°C ; [0003] Density: ...
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