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Cyclization/hydrolysis section micro-channel reaction method and reaction system in preparation of acesulfame potassium

A technology of acesulfame potassium and microchannel reaction, which is applied in organic chemistry and other fields, and can solve the problems of heavy ice machine load, high production cost, and many side reactions

Active Publication Date: 2020-07-07
NANTONG ACETIC ACID CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The present invention mainly aims at the problems of many side reactions in the cyclization / hydrolysis section in the preparation of acesulfame potassium, large ice machine load and high production cost, and develops a microchannel for the cyclization / hydrolysis section in the preparation of acesulfame potassium Response method

Method used

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  • Cyclization/hydrolysis section micro-channel reaction method and reaction system in preparation of acesulfame potassium
  • Cyclization/hydrolysis section micro-channel reaction method and reaction system in preparation of acesulfame potassium

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Experimental program
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Effect test

Embodiment 1

[0046] DKA reaction solution (10w%) and cyclizing agent SO 3 (15w%) solution enters the cyclization microreactor at the same time according to the volume ratio of 1:1, then enters the primary hydrolysis microreactor through the cyclization micro heat exchanger, and then passes through the primary hydrolysis micro heat exchanger and the secondary hydrolysis microreaction The acesulfame solution was obtained after the secondary hydrolysis micro-heat exchanger; the cyclization reaction temperature was controlled at -10°C, the pressure was 2MPa, and the residence time was 0.01s; the primary hydrolysis temperature was controlled at -10°C, the pressure was 2MPa, The residence time is 0.01s; the secondary hydrolysis temperature is controlled at 10°C, the pressure is 2MPa, and the residence time is 0.01s. The cyclohydrolysis yield was analyzed to be 92%, and the sugar content of the finished product AK was 99.5%.

Embodiment 2

[0048] DKA reaction solution (25w%) and cyclizing agent SO 3 (50w%) solution enters the cyclization microreactor at the same time according to the volume ratio of 1:2, then enters the primary hydrolysis microreactor through the cyclization micro heat exchanger, and then passes through the primary hydrolysis micro heat exchanger and the secondary hydrolysis microreaction Acesulfame solution was obtained after the secondary hydrolysis micro-heat exchanger; the cyclization reaction temperature was controlled at 60°C, the pressure was 9MPa, and the residence time was 15min; the primary hydrolysis temperature was controlled at 10°C, the pressure was 10MPa, and the residence time was 15min; the secondary hydrolysis temperature is controlled at 50°C, the pressure is 10MPa, and the residence time is 10min. The cyclohydrolysis yield was analyzed to be 93.2%, and the sugar content of the finished product AK was 99.4%.

Embodiment 3

[0050] DKA reaction solution (15w%) and cyclizing agent SO 3 (25w%) solution enters the cyclization micro-reactor at the same time according to the volume ratio of 1:1.5, then enters the primary hydrolysis micro-reactor through the cyclization micro-heat exchanger, and then passes through the primary hydrolysis micro-heat exchanger and the secondary hydrolysis micro-reaction The acesulfame solution was obtained after the secondary hydrolysis micro-heat exchanger; the cyclization reaction temperature was controlled at 35°C, the pressure was 5MPa, and the residence time was 7.5min; the primary hydrolysis temperature was controlled at 5°C, the pressure was 5MPa, and the residence time was 7.5s; the secondary hydrolysis temperature is controlled at 30°C, the pressure is 5MPa, and the residence time is 7.5min. The cyclohydrolysis yield was analyzed to be 93.5%, and the sugar content of the finished product AK was 99.4%.

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Abstract

The invention discloses a cyclization / hydrolysis section micro-channel reaction method and a cyclization / hydrolysis section micro-channel reaction system in preparation of acesulfame potassium. An acetyl acetamido sulfonic acid triethylamine (DKA) reaction liquid and a cyclizing agent solution simultaneously enter a cyclizing micro-reactor according to the volume ratio of 1: (1-2), then the reaction product enters a primary hydrolysis micro-reactor through a cyclizing micro-heat exchanger, and finally the hydrolysis product passes through a primary hydrolysis micro-heat exchanger, a secondaryhydrolysis micro-reactor and a secondary hydrolysis micro-heat exchanger to obtain an acesulfamic acid solution; wherein the cyclization reaction temperature is controlled to be -10 DEG C to 60 DEG C,the pressure is 0.1 MPa to 10 MPa, and the retention time is 0.01 s to 15 min; the primary hydrolysis temperature is controlled to be -10 DEG C to 10 DEG C, the pressure is 0.1 MPa to 10 MPa, and theretention time is 0.01 s to 10 min; and the secondary hydrolysis temperature is controlled to be 10-50 DEG C, the pressure is 0.1-10 MPa, and the retention time is 0.01s to 10 min. Cyclization / hydrolysis is integrated, side reactions are reduced through two-time hydrolysis, the load of an ice maker is reduced, and the product quality is improved.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of acesulfame potassium. Background technique [0002] AK sugar (Acesulfame-K), the chemical name is 6-methyl 1,2,3-oxathiazin-4(3)-one-2,2-potassium dioxide, commonly known as acesulfame-K English name: 6-Methyl -1,2,3-oxathiazin-4(3H)-one 2,2-dioxide potassium salt [0003] Appearance properties: colorless crystal [0004] Solubility: easily soluble in water, the solubility is 27 grams at 20°C [0005] CAS number: 55589-62-3 [0006] Molecular formula: C 4 h 4 o 4 KNS [0007] [0008] Molecular weight: 201.24 [0009] Melting point (°C): 229-232 [0010] Relative density (water=1): 1.81 [0011] pH: pH=5.5-7.5 [0012] Function and use: Acesulfame K has the advantages of safety, non-toxicity, stable property, sweet taste, no bad aftertaste, and reasonable price. It is one of the most stable sweeteners in the world. It is used in food, medici...

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