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Method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F

A technology of CH3SO2F and trifluoromethylsulfonyl fluoride, applied in organic chemistry, electrolysis process, electrolysis components, etc., can solve the problems of reducing the current efficiency of electrochemical fluorination products, difficulty in product separation and purification, and safety, etc. The effect of improved safety and reliability, safe and reliable process, and convenient preparation

Active Publication Date: 2010-06-23
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually in hydrogen fluoride HF and CH 3 SO 2 F contains a certain amount of moisture, so the current preparation method has the following defects: due to directly entering the electrochemical fluorination reactor, this will not only reduce the current efficiency of the electrochemical fluorination product; 2 O to generate OF during electrochemical fluorination 2 and other strong oxidative by-products, resulting in difficulties in the separation and purification of products and corrosion of equipment, as well as potential safety hazards in the operation process

Method used

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  • Method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F
  • Method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F

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Embodiment 1

[0019] As shown in the figure, a methanesulfonyl fluoride CH 3 SO 2 Preparation of trifluoromethanesulfonyl fluoride CF by electrochemical fluorination of F 3 SO 2 The method of F, described method step is as follows:

[0020] (1) Electrochemical method to remove water in hydrogen fluoride HF: add hydrogen fluoride HF in the flat-plate electrochemical reactor 1 that the anode material is Ni wire, the cathode material is Ni plate, and the distance between the cathode and the anode is 2mm, and the electrochemical reaction The operating voltage of device 1 is 4.0V~8.2V, the operating temperature of electrochemical reaction is -10℃~10℃, and the operating absolute pressure is 0.1MPa~1.0MPa for electrochemical dehydration reaction. When the operating voltage of electrochemical reaction reaches 8.2V, the apparent Operating current density≤1.0mA / cm 2 , indicating that the dehydration reaction is basically completed, and the anhydrous HF after dehydration is used as the third step ...

Embodiment 2

[0024] As shown in the figure, a methanesulfonyl fluoride CH 3 SO 2 Preparation of trifluoromethanesulfonyl fluoride CF by electrochemical fluorination of F 3 SO 2 The method of F, described method step is as follows:

[0025] (1) Electrochemical method to remove water in hydrogen fluoride HF: add hydrogen fluoride HF in the fixed bed electrochemical reactor 1 that the anode material is a Ni plate, the cathode material is a Ni plate, and the distance between the cathode and the anode is 8mm. The operating voltage of device 1 is 4.0V~8.2V, the operating temperature of electrochemical reaction is -10℃~10℃, and the operating absolute pressure is 0.1MPa~1.0MPa for electrochemical dehydration reaction. When the operating voltage of electrochemical reaction reaches 8.2V, the apparent Operating current density≤2.0mA / cm 2 , indicating that the dehydration reaction is basically completed, and the anhydrous HF after dehydration is used as the third step CH 3 SO 2 The reactant of F...

Embodiment 3

[0029] As shown in the figure, a methanesulfonyl fluoride CH 3 SO 2 Preparation of trifluoromethanesulfonyl fluoride CF by electrochemical fluorination of F 3 SO 2 The method of F, described method step is as follows:

[0030] (1) Electrochemical method removes the water in the hydrogen fluoride HF: add hydrogen fluoride HF in the plate type electrochemical reactor 1 that the anode material is a low-carbon steel plate, the cathode material is a low-carbon steel plate, and the distance between the cathode and the anode is 8mm. The operating voltage of the chemical reactor 1 is 4.6V-8.0V, the operating temperature of the electrochemical reaction is -10°C-10°C, and the operating absolute pressure is 0.1MPa-1.0MPa for the electrochemical dehydration reaction. When the operating voltage of the electrochemical reaction reaches 8.2V, Apparent operating current density≤1.0mA / cm 2 , indicating that the dehydration reaction is basically completed, and the anhydrous HF after dehydrat...

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Abstract

The invention relates to a method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F, the steps of the method are as follows: (1) water in HF is dehydrated through electrochemical method, and the anhydrous HF after dehydration is used as the reactant of CH3SO2F fluoridation at the third step and the solvent of the electrolyte; (2) water in the methanesulfonyl fluoride CH3SO2F is dehydrated through electrochemical method, and the anhydrous CH3SO2F after dehydration is used as the reactants of the electrochemical fluorination reaction at the third step; (3) for the anhydrous HF obtained at the first step and the anhydrous methanesulfonyl fluoride CH3SO2F obtained at the second step, the electrochemical fluorination reaction is conducted, gas-phase outlets of an electrochemical reactor 3 are trifluoromethyl sulfuryl fluoride CF3SO2F, hydrogen H2 and mixture formed through HF volatilization. The advantages of the invention are as follows: the preparation method is simple, the current efficiency of the product of electrochemical fluorination and the safety during the fluorination operation procedure are increased.

Description

technical field [0001] The invention relates to a method for preparing trifluoromethanesulfonyl fluoride CF 3 SO 2 The method of F, in particular a methanesulfonyl fluoride CH 3 SO 2 Preparation of trifluoromethanesulfonyl fluoride CF by electrochemical fluorination of F 3 SO 2 The method of F belongs to the field of fine chemical technology. Background technique [0002] Methylsulfonyl fluoride CH 3 SO 2 F is the direct electrochemical fluorination reaction in anhydrous HF to generate trifluoromethylsulfonyl fluoride CF 3 SO 2 F, trifluoromethanesulfonyl fluoride CF 3 SO 2 F is an important raw material for the synthesis of ionic liquids, fluorosurfactants and lithium-ion electrolytes, and has broad application prospects. The development and preparation of trifluoromethylsulfonyl fluoride CF 3 SO 2 F's new process methods and key technologies are important research and development areas for building functional, fine, and high-efficiency fine fluorine chemical pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/08C07C309/80C25B3/28
Inventor 许坚许文林陶荣辉王雅琼朱慧沙红霞任海吴彬赵世勇
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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