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Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F

A technology of CH3SO2F and methylsulfonyl fluoride, which is applied in the field of analysis and measurement of gas phase products of electrochemical fluorination of methanesulfonyl fluoride CH3SO2F, can solve the problems of long time required and many operation steps, and achieve less loss and high determination The effect of reliable data and simple reagents

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

This method uses many operation steps, takes a long time, and can only obtain the average current efficiency and average yield of the electrochemical fluorination process. Therefore, it has been an unsolved problem to invent a reliable and effective analytical method for on-line detection. technical problems

Method used

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  • Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F
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  • Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F

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Experimental program
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Embodiment 1

[0031] As shown in the figure, a methanesulfonyl fluoride CH 3 SO 2 The analysis and determination method of F electrochemical fluorination gas phase product, described method step is as follows:

[0032] (1) Cooling and condensation: In the indirect cooling heat exchanger, it will mainly contain trifluoromethanesulfonyl fluoride CF 3 SO 2 F, hydrogen fluoride HF and hydrogen H 2 methanesulfonyl fluoride CH 3 SO 2 The gas phase product of F electrochemical fluorination is cooled and condensed, the operating absolute pressure is 0.8MPa, cooled to -9°C, and the hydrogen fluoride HF in the gas phase is condensed into a liquid phase;

[0033](2) Gas-liquid separation: In the gas-liquid separator, the liquid phase hydrogen fluoride HF is returned to CH 3 SO 2 Recycling in F electrochemical fluorination reaction, containing trifluoromethanesulfonyl fluoride CF 3 SO 2 F and hydrogen H 2 The gas phase enters the next step;

[0034] (3) Chemical absorption: the gas phase mat...

Embodiment 2

[0038] As shown in the figure, a methanesulfonyl fluoride CH 3 SO 2 The analysis and determination method of F electrochemical fluorination gas phase product, described method step is as follows:

[0039] (1) Cooling and condensation: In the indirect cooling heat exchanger, it will mainly contain trifluoromethanesulfonyl fluoride CF 3 SO 2 F, hydrogen fluoride HF and hydrogen H 2 methanesulfonyl fluoride CH 3 SO 2 The gas phase product of F electrochemical fluorination is cooled and condensed, the operating absolute pressure is 0.5MPa, cooled to -15°C, and the hydrogen fluoride HF in the gas phase is condensed into a liquid phase;

[0040] (2) Gas-liquid separation: In the gas-liquid separator, the liquid phase hydrogen fluoride HF is returned to CH 3 SO 2 Recycling in F electrochemical fluorination reaction, containing trifluoromethanesulfonyl fluoride CF 3 SO 2 F and hydrogen H 2 The gas phase enters the next step;

[0041] (3) Chemical absorption: the gas phase m...

Embodiment 3

[0045] As shown in the figure, a methanesulfonyl fluoride CH 3 SO 2 The analysis and determination method of F electrochemical fluorination gas phase product, described method step is as follows:

[0046] (1) Cooling and condensation: In the indirect cooling heat exchanger, it will mainly contain trifluoromethanesulfonyl fluoride CF 3 SO 2 F, hydrogen fluoride HF and hydrogen H 2 methanesulfonyl fluoride CH 3 SO 2 The gas phase product of F electrochemical fluorination is cooled and condensed, the operating absolute pressure is 0.1MPa, cooled to -20°C, and the hydrogen fluoride HF in the gas phase is condensed into a liquid phase;

[0047] (2) Gas-liquid separation: In the gas-liquid separator, the liquid phase hydrogen fluoride HF is returned to CH 3 SO 2 Recycling in F electrochemical fluorination reaction, containing trifluoromethanesulfonyl fluoride CF 3 SO 2 F and hydrogen H 2 The gas phase enters the next step;

[0048] (3) Chemical absorption: the gas phase m...

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Abstract

The invention relates to an analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F, the steps of the method are as follows: (1) the gas-phase product of the CH3SO2F electrochemical fluorination is cooled and condensed, the HF in gas-phase is condensed to the HF in liquid-phase; (2) gas-liquid separation: the gas-phase product enters into the next step; (3) chemical absorption: the chemical absorbent is adopted, the acidic gas in the gas-phase product in the last step and the generated OF2 are neutralized and then are removed; (4) the gas-liquid separation: the gas-phase further enters a sampling analyzer of the gas chromatography; (5) chromatographic analysis: the gas-phase product gained at the last step enters a sample injector of the gas chromatography for analyzing and detecting, and then the relative molar percentage content of the CH3SO2F and H2 in the gas-phase product is obtained. The advantages of the invention are as follows: the operating procedure is simple, fast, the cost is low, on-site quantitative analyzing and detecting can be conducted, and the detected data is reliable.

Description

technical field [0001] The present invention relates to a kind of methylsulfonyl fluoride CH 3 SO 2 F The method for analyzing and measuring gas phase products of electrochemical fluorination belongs to the technical field of fine chemical industry. Background technique [0002] Methylsulfonyl fluoride CH 3 SO 2 Electrochemical fluorination of F in anhydrous hydrogen fluoride HF to generate trifluoromethylsulfonyl fluoride CF 3 SO 2 F, methylsulfonyl fluoride CH 3 SO 2 Preparation of trifluoromethanesulfonyl fluoride CF by electrochemical fluorination of F 3 SO 2 F is the important synthetic CF 3 SO 2 Method F, Trifluoromethanesulfonyl Fluoride CF 3 SO 2 F is an important raw material for the synthesis of other fine chemical fluorine-containing organic compounds, trifluoromethylsulfonyl 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 de...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 许文林陶勤艳王雅琼李建中司宗飞杨升沙红霞瞿燕芳赵世勇
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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