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Synthetic method of perfluoroalkyl sultone

A technology of perfluoroalkyl and synthetic methods, applied in chemical instruments and methods, chemical/physical/physical chemical processes, organic chemistry, etc., can solve the problems of long reaction time, etc. The effect of continuous production

Inactive Publication Date: 2020-04-28
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, the reaction temperature can be precisely controlled to avoid local overheating caused by the exothermic reaction, realize the combination of the reaction process and the aging process, and improve the conversion rate of dodecylbenzene, but the reaction time is too long

Method used

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  • Synthetic method of perfluoroalkyl sultone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The raw materials sulfur trioxide and tetrafluoroethylene were respectively metered by metering pumps and then continuously entered into the micro-mixer (Labtrix@ R After mixing in S1), enter the microreactor (Labtrix@ R The continuous reaction is carried out in S1), the channel equivalent diameter of the micromixer is 30 μm, and the channel equivalent diameter of the microreactor is 200 μm. The molar ratio of sulfur trioxide and tetrafluoroethylene is 1:1.1, the reaction temperature is 45°C, the reaction pressure is 0.2MPa, and the residence time is 8min; after the reaction, the temperature is lowered, and the liquid product obtained is purified by distillation. , Tetrafluoroethane-β-sultone with a purity of more than 99.2% can be obtained.

Embodiment 2

[0030] The raw materials sulfur trioxide and tetrafluoroethylene are respectively metered by a metering pump and then continuously enter the micro-mixer (Kunshan Fuxi Engineering Technology Co., Ltd., T-type mixer) for mixing, then enter the micro-reactor (Corning, G1) for continuous reaction , the channel equivalent diameter of the micromixer is 70 μm, and the channel equivalent diameter of the microreactor is 200 μm. The molar ratio of sulfur trioxide and tetrafluoroethylene is 1:1.2, the reaction temperature is 50°C, the reaction pressure is 0.3MPa, and the residence time is 10min; after the reaction, the temperature is lowered, and the liquid product obtained is purified by distillation. , Tetrafluoroethane-β-sultone with a purity of more than 99.4% can be obtained.

Embodiment 3

[0032] The raw materials sulfur trioxide and hexafluoropropylene are respectively metered by a metering pump and then continuously entered into a micro-mixer (Kunshan Fuxi Engineering Technology Co., Ltd., Y-type mixer) for mixing, and then enter a micro-reactor (Corning, G1) for continuous reaction , the channel equivalent diameter of the micromixer is 20 μm, and the channel equivalent diameter of the microreactor is 200 μm. The molar ratio of sulfur trioxide and tetrafluoroethylene is 1:1.3, the reaction temperature is 55°C, the reaction pressure is 0.45MPa, and the residence time is 12min; after the reaction is completed, the temperature is lowered, and after gas-liquid separation, the obtained liquid product is distilled and purified , Hexafluoropropane-β-sultone with a purity of more than 99.3% can be obtained.

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Abstract

The invention discloses a synthetic method of perfluoroalkyl sultone. The preparation method comprises the following steps: continuously introducing sulfur trioxide and perfluoroolefin into a micro-mixer for mixing; entering into a microreactor for reaction, wherein the molar ratio of sulfur trioxide to perfluoroolefin is 1: (1-1.5), the reaction temperature is 30-80 DEG C, the reaction pressure is 0.1-0.7 MPa, the retention time is 1.5-15 minutes, cooling after the reaction is finished and performing gas-liquid separation, and distilling and purifying the obtained liquid productto obtain theperfluoroalkyl sultone product. By utilizing the efficient mass transfer and heat transfer characteristics of the micro-mixer and the micro-reactor, the operation process of perfluoroalkyl sultone synthesis is simplified, the reaction time is shortened, the continuous reaction is realized, and the safety of the equipment in the operation process is improved; meanwhile, the method has the advantages of high reaction yield, few by-products and easiness in subsequent enlarged production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing perfluoroalkyl sultones. Background technique [0002] Perfluoroalkyl sultone is a special fluorine-containing fine chemical and an important fluorine-containing intermediate, which can be used to prepare functional compounds containing carboxyl or sulfonic acid groups, among which tetrafluoroethane-β-sultone is the most widely used A broad class of perfluoroalkyl sultones. Due to its special structure, perfluoroalkyl sultone can react with various olefins, cycloalkanes, nucleophiles, etc. to synthesize fluorine-containing compounds of various structures, and is mainly used in the synthesis of functional polymer materials and fine chemistry Products, such as PSVE, fluorine-containing surfactants and fluorine grease, etc. [0003] At present, perfluoroalkyl sultones are mainly prepared by the addition reaction of sulfur trioxide and perfluoroolefins. F...

Claims

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Application Information

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IPC IPC(8): C07D327/04B01J19/00
CPCB01J19/0093C07D327/04
Inventor 马利勇叶立峰张坚文刘华平郑佳
Owner JUHUA GROUP TECH CENT
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