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Method for preparing fluoro olefin

A technology of fluoroolefins and fluorovinyl sulfate, applied in the field of fluorine-containing fine chemicals, can solve the problems of low monomer yield, complicated preparation process, and low yield

Active Publication Date: 2010-10-06
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent US.3282875 is the earliest preparation of alkylene ether monomers containing sulfonyl fluoride groups announced by DuPont, which is carried out by high-temperature cracking; U.S. Patent US.3560568 is a short-chain The preparation of alkylene ether monomers containing sulfonyl fluoride groups in the structure adopts the method of ring-opening isomerization, and the final monomer yield is very low; US Patent US. The process of oxychloropropane addition and pyrolysis prepares alkylene ether monomers containing sulfonyl fluoride groups, but the preparation process of this pentafluoroepichlorohydrin is very complicated and the yield is not high

Method used

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  • Method for preparing fluoro olefin
  • Method for preparing fluoro olefin
  • Method for preparing fluoro olefin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Clean and fully dry the 10L stainless steel high-pressure reactor equipped with a circulating cooling / heating system, temperature control system, and feeding system, then vacuumize it, fill it with nitrogen and replace it three times until the oxygen content is controlled below 10ppm, and then vacuumize it to -0.1MPa. Add 760g cesium fluoride, 580g potassium fluoride, solvent tetraethylene glycol dimethyl ether 2Kg, trifluorovinyl sulfate 1965g in the system, solvent consumption is 101.8% of trifluorovinyl sulfate total mass, catalyst consumption The number of moles is 1.5 times of the total molar amount of trifluorovinyl sulfate added, and the stirring temperature is controlled at 25°C, and tetrafluorosultone (molecular formula: FO 2 SCF 2 COF) 1800g, just keep the temperature at 25±1°C. After the dropwise addition, stir at constant temperature for two hours, stop stirring, lower the temperature, let it stand for stratification, and pass the lower layer of colorless an...

Embodiment 2

[0031] Clean and fully dry the 10L stainless steel high-pressure reactor equipped with a circulating cooling / heating system, temperature control system, and feeding system, then vacuumize it, fill it with nitrogen and replace it three times until the oxygen content is controlled below 10ppm, and then vacuumize it to -0.1MPa. In the system, add 304g cesium fluoride, 580g potassium fluoride, solvent adiponitrile 2Kg, trifluorovinyl sulfate 1965g, solvent consumption is 101.8% of trifluorovinyl sulfate total mass, and the mole number of catalyst consumption is Add 1.2 times the total molar amount of trifluorovinyl sulfate, stir and control the temperature at 15°C, slowly add the monoaddition product of tetrafluorosultone and hexafluoropropylene oxide (molecular formula: FO 2 SCF 2 CF 2 OCF (CF 3 ) COF) 3460g, the temperature can be controlled at 15±1°C. After the dropwise addition is completed, stir at a constant temperature for two hours, stop stirring, cool down, stand for st...

Embodiment 3

[0034] Clean and fully dry the 10L stainless steel high-pressure reactor equipped with a circulating cooling / heating system, temperature control system, and feeding system, then vacuumize it, fill it with nitrogen and replace it three times until the oxygen content is controlled below 10ppm, and then vacuumize it to -0.1MPa. Add 608g cesium fluoride, 522g potassium fluoride into the system, solvent tetraethylene glycol dimethyl ether 1Kg, acetonitrile 1Kg, trifluorovinyl sulfate 1965g, solvent consumption is 101.8% of the total mass of trifluorovinyl sulfate %, the molar number of the catalyst consumption is 1.3 times of the total molar amount of the added trifluorovinyl sulfate ester, stirring and temperature control is at 10 ℃, slowly dripping 3-acyl fluoride-propanesulfonyl fluoride ( Molecular formula: FO 2 SCF 2 CF 2 COF) 2300g, the temperature can be controlled at 10±1°C. After the dropwise addition is completed, stir at a constant temperature for two hours, stop stir...

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Abstract

The invention discloses a method for preparing fluoro olefin, which comprises that: a perfluoro straight chain or branched chain acyl fluoride compound reacts with trifluoro vinyl ethyl sulfate in an organic solvent under the action of a catalyst so as to form a product having a general formula shown by the formula (I). The method avoids a pyrolysis route and uses no unconventional monomers, the used trifluoro vinyl ethyl sulfate can be prepared at a yield of above 95 percent, and a fluoro olefin monomer is prepared easily through an addition reaction, and a high-purity monomer can be obtained through rectification. CF2=CF-O-Rf (I).

Description

technical field [0001] The invention belongs to the field of fluorine-containing fine chemicals, and relates to a preparation method of a class of fluoroolefins, which are used to synthesize fluororesins with proton exchange functions. Background technique [0002] Since the application of perfluorosulfonic acid ion exchange membranes in the chlor-alkali industry and proton exchange membrane fuel cells in the 1970s, perfluorosulfonic acid ion exchange membranes have been extensively studied in various countries around the world. The use of fluorine-containing or non-fluorine ion exchange membranes in electrolysis cells and fuel cells is well known. Such ionic membranes have bonded anions and bonded cations for cation exchange. The ionic membrane divides the battery or electrolytic cell into a cathode chamber and an anode chamber, through which ions can selectively pass. Although many polymers can be used as ion exchange membranes, it has been proven that fluorine-containin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/82C07C303/22
Inventor 张永明魏茂祥秦胜高自宏
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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