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Method for preparing fluoroalkyl vinyl ether

A technology of fluoroalkyl alkenyl ether and trifluorovinyl sulfate, which is applied in the field of fluorine-containing fine chemicals and can solve the problems of chlorine gas and caustic soda current efficiency decline and the like

Active Publication Date: 2010-04-21
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

Practice has proved that perfluorinated ion-exchange membranes containing ion-exchange groups, especially sulfonic acid groups and carboxylic acid groups, are more suitable for use as composite ion-exchange membranes for chlor-alkali electrolyzers due to their resistance to chemical degradation. The perfluorocarboxylic acid layer exchange membrane mainly prevents the reverse migration of hydroxyl anions into the anode chamber. Once the reverse migration of hydroxyl anions enters the anode chamber, the current efficiency of chlorine gas and caustic soda will be greatly reduced.

Method used

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  • Method for preparing fluoroalkyl vinyl ether
  • Method for preparing fluoroalkyl vinyl ether
  • Method for preparing fluoroalkyl vinyl ether

Examples

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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. In the system, add 1368g cesium fluoride, 522g potassium fluoride, solvent tetraethylene glycol dimethyl ether 1Kg, acetonitrile 1Kg, trifluorovinyl sulfate 2950g, solvent consumption is 67.8% of trifluorovinyl sulfate total mass, The molar number of catalyst consumption is 1.2 times of the total molar amount of the added trifluorovinyl sulfate, and the stirring temperature is controlled at 10° C., and slowly drips 3-methyl carbocarboyl perfluoropropionyl fluoride (molecular formula: CH 3 OOCCF 2 COF) 2340g, the temperature can be controlled at 10±1°C. After the dropwise addition, stir at constant temperature for two hours, stop stirring, cool down, let s...

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 3040g cesium fluoride, solvent tetraethylene glycol dimethyl ether 2.5Kg, trifluorovinyl sulfate 2950g, solvent consumption is 84.75% of trifluorovinyl sulfate total mass, and the mole number of catalyst consumption is Added 1.33 times the total molar amount of trifluorovinyl sulfate, stirred and controlled the temperature at 15°C, and slowly added 4-methoxycarboxybutyryl fluoride (molecular formula: CH 3 OOCCF 2 CF 2 COF) 3090g, just keep the temperature at 15±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 c...

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. In the system, add 1064g cesium fluoride, 464g potassium fluoride, solvent tetraethylene glycol dimethyl ether 1.3Kg, adiponitrile nitrile 1.2Kg, trifluorovinyl sulfate 1965g, solvent consumption is the total amount of trifluorovinyl sulfate 127.2% of the mass, the molar amount of the catalyst is 1.5 times of the total molar amount of trifluorovinyl sulfate added, stirring and controlling the temperature at 20°C, and slowly adding 6-methylcarboxyperfluoropropane dropwise through the feeding system Oxypropionyl fluoride (molecular formula: CH 3 OOCCF 2 CF 2 OCF (CF 3) COF) 3220g, the control temperature can be kept between 20±1°C, after the dropwise addi...

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Abstract

The invention discloses a method for preparing fluoroalkyl vinyl ether. The method comprises the following steps of reacting a perfluor linear chain or branched chain compound with trifluoropropylmethyl sulfuric ester in an organic solvent under the action of a catalyst to form a product having a general formula shown in the formula (I). A high-temperature cracking route is avoided being used, unconventional monomers are not used, and the used trifluoropropylmethyl sulfuric ester can be prepared by a yield being more than 95 percent. Fluoro olefin monomers are easier prepared through an addition reaction, and high-purity monomers can be obtained through rectification. The general formula is 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 fluoroalkylene ethers, which are widely used in the synthesis of fluororesins with proton exchange functions, and membrane products prepared from such fluororesins It is used in the composite membrane diaphragm of electrolytic cells in the chlor-alkali industry to transport protons and prevent the reverse migration of hydroxyl radicals from the cathode chamber to the anode chamber. Background technique [0002] Since the ionic membrane electrolysis method was applied in the chlor-alkali industry in the 1970s, this technology has become the development direction of the technical transformation of old factories in the chlor-alkali industry and the development of new electrolysis devices. The use of fluorine-containing ion exchange membranes in electrolytic cells is well known. Such ionic membranes have bonded anions and bonded cati...

Claims

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Application Information

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IPC IPC(8): C07C69/734C07C67/31
Inventor 秦胜高自宏魏茂祥李勇
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD