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Method for preparing perfluoromethyl vinyl ether

A technology of fluoromethyl vinyl ether and methoxypropionic acid, which is applied in the field of preparation of perfluoromethyl vinyl ether, can solve the problems such as the corrosiveness of the reactor, which is unfavorable for industrialized scale-up production and the like, and achieves environmental friendliness, Continuous production process, high yield effect

Active Publication Date: 2019-03-05
SINOCHEM MODERN ENVIRONMENTAL CHEM INDAL XI ANCO +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second step of this method requires the use of highly explosive tetrafluoroethylene and the reaction must be carried out in an oxygen-free environment, which has great potential safety hazards
At the same time, due to the addition of water in the second step of the reaction, the free metal fluoride salt formed is corrosive to the reactor, which is not conducive to industrial scale-up production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Accurately weigh 200ml of polar aprotic organic solvent diethylene glycol dimethyl ether, 5g of titanium tetraethoxide as the main catalyst, and 200g of 2-methoxypropanol, add them to a 1L stainless steel autoclave reactor, replace with nitrogen, and vacuumize , under stirring and maintaining a temperature of about 25 ° C for 30 min. Lower the temperature to -5°C to 0°C, and continuously add 500 g of perfluoro-2-methoxypropionyl fluoride at a rate of 5 ml / min to 30 ml / min. Esterification begins with temperature rise, the temperature is maintained at 80°C, and the pressure is ≤1.5MPa. After 8 hours of reaction, 600 g of the product was collected. After analysis, the product was heptafluoro-2-methoxypropionic acid-5-methoxypropyl ester with a purity of ≥99%. The reaction yield of this step is ≥95%.

[0048] Add 600 g of heptafluoro-2-methoxypropionic acid-5-methoxypropyl ester and 100 g of diethylene glycol dimethyl ether into a 3L stainless steel autoclave reactor, re...

Embodiment 2

[0052] Accurately weigh 200ml of diethylene glycol dimethyl ether as a polar aprotic organic solvent, 5g of titanium tetra-n-propoxide as the main catalyst, and 150g of 2-methoxypropanol, add them to a 1L stainless steel autoclave reactor, and replace with nitrogen. Vacuumize and maintain the temperature at about 25°C for 30min under stirring. Lower the temperature to 0°C to 10°C, and continuously add 500 g of perfluoro-2-methoxypropionyl fluoride at a rate of 5 ml / min to 15 ml / min. The temperature was raised for esterification, the temperature was maintained at 90°C, and the pressure was ≤1.5MPa. After 8 hours of reaction, 470g of the product was collected. After analysis, the product was (heptafluoro-2-methoxypropionic acid-5-methoxypropyl ester), and the purity was ≥99%. The reaction yield of this step is ≥95%.

[0053] Add 470g (heptafluoro-2-methoxypropionic acid-5-methoxypropyl ester) and solvent diethylene glycol dimethyl ether 200g into a 3L stainless steel autoclave...

Embodiment 3

[0057] Accurately weigh 200ml of tetraglyme, a polar aprotic organic solvent, 10g of main catalyst zinc oxide, and 150g of 2-methoxypropanol, and add them to a 1L stainless steel autoclave reactor, replace with nitrogen, vacuumize, and stir Lower and maintain the temperature at about 25°C for 30min. Lower the temperature to 0°C to 10°C, and continuously add 600g of perfluoro-2-methoxypropionyl fluoride at a rate of 10ml / min to 30ml / min. The temperature was raised for esterification, the temperature was maintained at 80°C, and the pressure was ≤1.5MPa. After 8 hours of reaction, 460g of the product was collected. After analysis, the product was (heptafluoro-2-methoxypropionic acid-5-methoxypropyl ester), and the purity was ≥99%. The reaction yield of this step is ≥95%.

[0058] Add 460g (heptafluoro-2-methoxypropionic acid-5-methoxypropyl ester) and solvent tetraglyme 200g into a 3L stainless steel autoclave reactor, replace with nitrogen, vacuumize, and pass into N 2 with ...

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PUM

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Abstract

The invention provides a three-step method for preparing perfluoromethyl vinyl ether. The method uses 2-methoxypropanol and perfluoro-2-methoxypropionyl fluoride as raw materials, and conducts an esterification reaction, a fluorination reaction and a thermal decomposition reaction to obtain the fluoromethyl vinyl ether. The method provided by the invention is stable in reaction conditions, easy for industrialized continuous production; and the product perfluoromethyl vinyl ether has high yield and high purity.

Description

technical field [0001] The invention relates to a preparation method of perfluoromethyl vinyl ether. Background technique [0002] Perfluoromethyl vinyl ether, abbreviated PMVE, chemical formula CF 3 OCF=CF 2 , is an important monomer that can be used to synthesize new high-efficiency pesticides and new fluoroplastics and fluororubbers with excellent comprehensive properties, such as perfluoroether rubber for low and high temperature resistance, acid and alkali resistance and corrosion resistance, new non-toxic High-efficiency insecticide difenfluramide and copolymerization with tetrafluoroethylene to prepare melt-processable fluororesin, etc. [0003] For the preparation method of perfluoromethyl vinyl ether, the prior art has the following reports: [0004] (1) U.S. Patent US3114778 reports a two-step method for preparing perfluoromethyl vinyl ether. First, carbonyl fluoride and hexafluoropropylene oxide are used as raw materials, and under the action of activated carbo...

Claims

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Application Information

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IPC IPC(8): C07C41/18C07C43/16
CPCC07C41/18C07C67/14C07C67/307C07C43/16C07C69/708
Inventor 马亚锋杨会娥魏攀许磊齐仲龙晏少华
Owner SINOCHEM MODERN ENVIRONMENTAL CHEM INDAL XI ANCO
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