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Method for electrochemically preparing trifluoromethylsulfonyl fluoride from methylsulfonyl chloride

A technology of electrochemistry of methylsulfonyl chloride and trifluoromethylsulfonyl, which is applied in the field of electrochemical preparation of trifluoromethylsulfonyl fluoride from methylsulfonyl chloride, can solve the problems of complex reaction, high cost, low safety and the like, To achieve the effect of simple preparation method, convenient operation and good safety

Active Publication Date: 2021-05-07
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) The preparation method is complicated: since there is no methylsulfonyl fluoride product on the market, if you want to prepare trifluoromethanesulfonyl fluoride with methylsulfonyl fluoride, you must first prepare the methylsulfonyl fluoride product, and then use Preparation of trifluoromethylsulfonyl fluoride products from methylsulfonyl fluoride; the above-mentioned preparation method prepares trifluoromethylsulfonyl fluoride from methylsulfonyl chloride through a two-step reaction; wherein, the methylsulfonyl fluoride prepared in step 1) The purity of fluorine is low, and it needs further purification before it can be used in the reaction of step 2) to prepare trifluoromethanesulfonyl fluoride, the reaction is complicated and the cost is relatively high
[0005] (2) This preparation method can produce a large amount of three wastes: there will be a small amount of potassium fluoride and the impurity produced by the hydrolysis of methanesulfonyl chloride in the potassium chloride aqueous solution that step 1) produces, and these impurities can't be recycled directly
[0006] (3) safety is lower: step 1) contains moisture in the methanesulfonyl fluoride of preparation, and the methanesulfonyl fluoride that step 1) makes can produce oxygen difluoride (OF) during step 2) electrolysis 2 ), it will cause the electrolytic tank to explode, and there is a potential safety hazard
[0007] (4) The energy consumption of electrolysis is relatively high: this preparation method completely removes the moisture in the electrolyte, requires long-term electrolytic dehydration, and consumes a large amount of electric energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Add 1kg methanesulfonyl chloride, 0.30kg lithium fluoride and 8.7kg anhydrous hydrogen fluoride in the electrolytic cell to form an electrolyte, the anode material used for electrolysis is nickel, and the cathode material is carbon steel;

[0033] (2) The temperature is controlled at -10°C, and the electrolytic dehydration is carried out at a voltage of 3.0V for 10 hours;

[0034] (3) Perform electrochemical fluorination reaction by electrolysis at a temperature of -10°C and a voltage of 5.5V to obtain electrolytic gas, which is analyzed by gas chromatography. The electrolytic gas produced by the anode contains trifluoromethanesulfonyl fluoride, and the yield is 90%. , the cathode produced hydrogen; judged by chemical method that the electrolytic reaction produced hydrogen chloride; the total volume of the electrolytic gas was 100%, and the volume fraction of trifluoromethanesulfonyl fluoride prepared in the present embodiment was 18%.

Embodiment 2

[0036] (1) Add 1kg methanesulfonyl chloride, 0.25kg antimony pentafluoride and 2.2kg anhydrous hydrogen fluoride in the electrolytic cell to form electrolyte, the anode material used in electrolysis is nickel alloy, and the cathode material is nickel;

[0037] (2) The temperature is controlled at 5°C, and the electrolytic dehydration is carried out for 5 hours at a voltage of 4.0V;

[0038] (3) Electrochemical fluorination reaction was carried out by electrolysis at a temperature of 10°C and a voltage of 6.2V to obtain electrolytic gas, which was analyzed by gas chromatography, and the electrolytic gas produced by the anode contained trifluoromethanesulfonyl fluoride, and the yield was 89%, The cathode produced hydrogen, and it was judged by chemical method that the electrolytic reaction produced hydrogen chloride; based on the total volume of the electrolytic gas as 100%, the volume fraction of trifluoromethanesulfonyl fluoride prepared in this example was 17.8%.

Embodiment 3

[0040] (1) Add 1kg methanesulfonyl chloride, 0.3kg Potassium Fluoride and 3.7kg anhydrous hydrogen fluoride in the electrolyzer, form electrolyte, the anode material that electrolysis adopts is nickel alloy, and cathode material is nickel alloy;

[0041] (2) The temperature is controlled at 20°C, and the electrolytic dehydration is carried out for 2 hours at a voltage of 4.5V;

[0042] (3) electrolysis at a temperature of 20° C. and a voltage of 7.5 V for electrochemical fluorination reaction to obtain electrolytic gas, which was analyzed by gas chromatography. The electrolytic gas produced by the anode contained trifluoromethanesulfonyl fluoride, and the yield was 91%. The cathode produced hydrogen, and it was judged by chemical method that the electrolytic reaction produced hydrogen chloride; based on the total volume of the electrolytic gas as 100%, the volume fraction of trifluoromethanesulfonyl fluoride prepared in this example was 18.2%.

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Abstract

The invention relates to a method for electrochemically preparing trifluoromethylsulfonyl fluoride from methylsulfonyl chloride, and belongs to the field of fine chemical engineering. The method comprises the following steps: adding methylsulfonyl chloride, a conductive agent and anhydrous hydrogen fluoride into an electrolytic bath to form an electrolyte; subjecting the electrolyte to electrolytic dehydration for 2-10 h under the conditions that the temperature ranges from -10 DEG C to 20 DEG C and the voltage ranges from 3 V to 4.5 V; and under the conditions that the temperature ranges from -10 DEG C to 20 DEG C and the voltage ranges from 5 V to 7.5 V, conducting eletrolysis to obtain electrolysis gas, wherein the electrolysis gas contains trifluoromethylsulfonyl fluoride. According to the method, methylsulfonyl chloride is used as a raw material, a conductive agent and anhydrous hydrogen fluoride are added, an electrochemical fluorination reaction is carried out at a constant voltage, trifluoromethylsulfonyl fluoride can be obtained, wherein the anhydrous hydrogen fluoride is a solvent and a fluorinating agent of the electrolyte. The electrochemical preparation method of trifluoromethylsulfonyl fluoride provided by the invention is simple and convenient to operate, low in cost and suitable for large-scale application.

Description

technical field [0001] The invention relates to a method for electrochemically preparing trifluoromethanesulfonyl fluoride from methanesulfonyl chloride, which belongs to the field of fine chemicals. Background technique [0002] Trifluoromethanesulfonyl fluoride (CF 3 SO 2 F) is an important raw material for fine chemical synthesis, and can be used to prepare products in related fields such as pharmaceutical intermediates, ionic liquids, lithium ion electrolytes, etc., and has a very wide application prospect. At present, trifluoromethanesulfonyl fluoride is mainly prepared by methylsulfonyl chloride, and its preparation method is: step 1) methylsulfonyl chloride is chemically fluorinated in potassium fluoride aqueous solution to generate methylsulfonyl fluoride, step 2) a The electrochemical fluorination of sulfonyl fluoride in anhydrous hydrogen fluoride produces trifluoromethylsulfonyl fluoride. [0003] The shortcoming of this preparation method has the following poi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/28C25B3/11C25B3/07C25B1/26
CPCC25B1/26
Inventor 朱姜涛范娜王斌吝子东李柄缘李林王志民张雷倪珊珊
Owner PERIC SPECIAL GASES CO LTD
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