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Environment-friendly synthesis method of high-yield perfluoromethylvinyl ether (PMVE)

A technology of perfluoromethyl vinyl ether and fluoromethyl vinyl ether, which is applied in the field of synthesis of special fluorine-containing comonomers, can solve the problems of high cost, complicated process, difficult acquisition of raw materials, etc., and achieves easy separation and reaction. The effect of high efficiency and high product yield

Active Publication Date: 2015-03-18
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of this method is complicated, the raw material of trifluoromethyl-1,1,2-trifluoro-1,2-dichloro-ethyl ether is difficult to obtain, and the cost is high, which is also unfavorable for large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Accurately weigh 33.0 g of potassium fluoride, dry and grind in a muffle furnace at 400° C. for 8 hours to remove crystal water therein. Using nitrogen protection, the potassium fluoride powder after strict water removal was put into a 5-liter dry reaction kettle. The reaction kettle is respectively connected to steel cylinders of carbonyl fluoride and hexafluoropropylene oxide (HFPO), and is equipped with a stirring device and a material exporting device.

[0036] Under the protection of nitrogen, the 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF 4 )liquid. The reaction kettle was cooled to 0°C, and the solution was vigorously stirred for 30 minutes.

[0037] Feed 0.5kg / h hexafluoropropylene oxide and 0.17kg / h carbonyl fluoride into the reactor, maintain the reaction temperature at -5-5°C, and feed for 5 hours. Continue to stir for 30 minutes after stopping feeding, and the reaction pressure is 0.5MPa.

[0038] The reacted product material was exported, p...

Embodiment 2

[0040] Accurately weigh 23.5 g of potassium fluoride, dry in a muffle furnace at 400°C for 8 hours and grind to remove crystal water therein. Using nitrogen protection, the potassium fluoride powder after strict water removal was put into a 5-liter dry reaction kettle. The reaction kettle is respectively connected to steel cylinders of carbonyl fluoride and hexafluoropropylene oxide (HFPO), and is equipped with a stirring device and a material exporting device. Under nitrogen protection, drop into the 1-butyl-3-methylimidazole tetrafluoroborate ([BMIM]BF of solvent tetraethylene glycol dimethyl ether 1500g and 7.5ml in the reactor 4)liquid. The reaction kettle was cooled to 3°C, and the solution was vigorously stirred for 30 minutes. Feed 0.5kg / h hexafluoropropylene oxide and 0.17kg / h carbonyl fluoride into the reactor, maintain the reaction temperature at -5-5°C, and feed for 4.5 hours. Continue to stir for 30 minutes after stopping feeding, and the reaction pressure is 0....

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Abstract

The invention relates to an environment-friendly synthesis method of high-yield perfluoromethylvinyl ether (PMVE). The method comprises the following steps: preparing an alkali metal fluoride, 1-butyl-3-methyl imidazolium tetrafluoroborate and a polarity organic solvent into a catalyst solution under nitrogen protection; reducing the temperature to be 0-5 DEG C, and uniformly stirring; introducing carbonyl fluoride and hexafluoropropylene oxide into the catalyst solution, and carrying out an addition reaction at the temperature of 10 DEG C below zero to 20 DEG C; introducing the obtained addition product into a cracking tower filled with carbonate for cracking, thereby obtaining the PMVE. The synthesis method is high in reaction efficiency and high in product yield, the solvent used in the reaction can be recycled, and the used ionic liquid promoter is easy to separate and is environmental friendly.

Description

technical field [0001] The present invention relates to a method for preparing perfluoromethyl vinyl ether, in particular to a method for preparing perfluoromethyl vinyl ether by reacting carbonyl fluoride with hexafluoropropylene oxide (HFPO), which belongs to special Technical field of fluorine-containing comonomer synthesis. Background technique [0002] Perfluoromethyl vinyl ether is a widely used fluorine-containing comonomer, usually used in the production of fluoroplastics, fluororubbers and fluoropolymers containing fluorine functional groups that can be thermoplastically processed. Excellent raw material for modification. For example, perfluoromethyl vinyl ether and tetrafluoroethylene are copolymerized to form fluororubber, which has a wide temperature range, chemical corrosion resistance and aging resistance without changing the traditional polytetrafluoroethylene. At the same time of performance, it also shows excellent processing performance, and at the same t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/17C07C41/18
CPCC07C41/18C07C51/62C07C43/17C07C59/135
Inventor 王汉利张琳涵王军
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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