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Analytical test method of perfluorosulfonyl fluoride alkene ether

The technology of perfluorosulfonyl fluoroalkenyl ether and fluorosulfonyl fluoroalkenyl ether is applied in the field of analysis and testing of perfluorosulfonyl fluoroalkenyl ether, which can solve the problems of quantitative analysis of impurities and products, and achieve reliable results and simple operation. Effect

Pending Publication Date: 2020-07-10
SAIC MOTOR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, high-purity perfluorosulfonyl fluoride alkenyl ether is required in production, but it is difficult to quantitatively analyze impurities and products using conventional chromatographic detection methods, nuclear magnetic resonance and infrared analysis.

Method used

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  • Analytical test method of perfluorosulfonyl fluoride alkene ether
  • Analytical test method of perfluorosulfonyl fluoride alkene ether
  • Analytical test method of perfluorosulfonyl fluoride alkene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Add 2ml of carbon tetrachloride and 1mmol of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride to a 10mL reaction test tube with magnetic stirring and heating bath (high-resolution NMR purity calibration concentration 98.50%), drop 1.1 mmol of liquid bromine, control the reaction temperature to 40 ° C, react for 0.2 hours, add 1 mmol of sodium bicarbonate aqueous solution to wash, separate layers, take the lower layer of liquid, and inject Agilent's 7890 chromatographic, chromatographic The column is DB-5, and the analytical purity is 98.49%.

Embodiment 2

[0047] Add 1ml of carbon tetrachloride and 1mmol of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride to a 10mL reaction tube with magnetic stirring and heating bath (high-resolution NMR purity calibration concentration 99.90%), 1.05mmol of liquid bromine was added dropwise, the reaction temperature was controlled to 40°C, and the reaction was carried out for 0.1 hour, adding 0.5mmol of sodium bicarbonate aqueous solution for washing, layering, taking the lower layer of liquid, and injecting Agilent's 7890 chromatogram, The chromatographic column is DB-5, and the analytical purity is 99.88%.

Embodiment 3

[0049] Add 1ml of carbon tetrachloride and 1mmol of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride to a 10mL reaction tube with magnetic stirring and heating bath (high-resolution NMR purity calibration concentration 99.95%), 1.05 mmol of liquid bromine was added dropwise, the reaction temperature was controlled to 40° C., and the reaction was carried out for 0.1 hour, adding 0.5 mmol of sodium bicarbonate aqueous solution for washing, layering, taking the lower layer of liquid, and injecting Agilent 7890 chromatogram, The chromatographic column is DB-5, and the analytical purity is 99.92%.

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Abstract

The invention provides an analytical test method of perfluorosulfonyl fluoride alkene ether, which comprises the following steps: mixing a perfluorosulfonyl fluoride alkene ether solution with a bromination reagent, reacting, washing the reaction product, and carrying out gas chromatographic analysis. According to the method, after the perfluorosulfonyl fluoride alkene ether is pretreated, the product purity can be quantitatively analyzed by adopting gas chromatography, the result is reliable, the operation is simple, and the method can be used for guiding the research and production of the perfluorosulfonyl fluoride alkene ether.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to an analysis and test method of perfluorosulfonyl fluoride alkenyl ether. Background technique [0002] Perfluorosulfonyl fluoride alkenyl ether is an important fluorine-containing intermediate, and its main function is to introduce functional sulfonic acid group chains into polymers. Perfluorosulfonyl fluoride alkenyl ether is the core raw material for the synthesis of perfluorosulfonic acid ion exchange resins. Perfluorosulfonic acid ion exchange resins are mainly used to synthesize perfluorosulfonic acid ion exchange membranes, and can also be used as super acid catalysts. The perfluorosulfonic acid ion exchange membrane was made of perfluorosulfonic acid ion exchange membrane by the chemical name of perfluoro(3,6-dioxa-4-methyl-7-octene)sulfonyl fluoride from DuPont of the United States. It was first developed and adopted in the 1970s. Widely used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 刘芳陈焱锋冯奇汪婉郁波李军巍
Owner SAIC MOTOR
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