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Method for preparing pentafluoride ethyl perfluoro isopropyl ketone through gas phases

A technology of perfluoroisopropyl ketone and pentafluoroethyl, which is applied in the field of gas phase preparation of pentafluoroethyl perfluoroisopropyl ketone, can solve the problems of difficulty in obtaining raw materials, many types of fragments, low yield and the like, and achieves high price low cost effect

Active Publication Date: 2018-07-24
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The above-mentioned prior art has the following problems: (1) the raw materials of the first route are difficult to obtain, and most of them have low yields; (2) there are too many types of fragments obtained by the pyrolysis of the second route, so that the selection of the target product is greatly reduced (3) The raw material of the third route is difficult to obtain, and the yield is extremely low; (4) Although the raw material is easy to obtain in the fourth route, it uses an organic solvent that is difficult to recover for liquid phase reaction, which is likely to cause serious pollution

Method used

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  • Method for preparing pentafluoride ethyl perfluoro isopropyl ketone through gas phases
  • Method for preparing pentafluoride ethyl perfluoro isopropyl ketone through gas phases
  • Method for preparing pentafluoride ethyl perfluoro isopropyl ketone through gas phases

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Experimental program
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Effect test

Embodiment 1

[0047] Fill 10 milliliters of the addition catalyst 10%CsF / 90%CrF that the above-mentioned method prepares in the tubular reactor made of Incon alloy of inner diameter 1 / 2 inch, long 30cm 3 . The reaction conditions are as follows: the reaction temperature is raised to 160°C, the molar ratio of hexafluoropropylene oxide to hexafluoropropylene is 1:1, the contact time is 0.25s, and the reaction pressure is 0.1MPa. The reaction product was collected by a sampling bag made of polytetrafluoroethylene. After 10 hours of reaction, a sample was taken from the sampling bag for GC analysis. The reaction result was: the conversion rate of hexafluoropropylene oxide was 100%, and the conversion rate of pentafluoroethyl perfluoro The selectivity of isopropyl ketone is 99.6%.

[0048] After rectification, high-purity pentafluoroethyl perfluoroisopropyl ketone was isolated, and the boiling point of pentafluoroethyl perfluoroisopropyl ketone was 49.2°C (pressure 760mmHg).

Embodiment 2

[0050] The isomerization catalyst 10%CsF / 90%AlF that 10 milliliters of above-mentioned methods are prepared is packed in the tubular reactor that inner diameter 1 / 2 inch, length 30cm make of Incon alloy 3 . The reaction conditions are as follows: the reaction temperature is raised to 140° C., the contact time of hexafluoropropylene oxide is 0.25 s, and the reaction pressure is 0.1 MPa. The reaction product was collected by a sampling bag made of polytetrafluoroethylene. After 10 hours of reaction, a sample was taken from the sampling bag for GC analysis. The reaction results were as follows: the conversion rate of hexafluoropropylene oxide was 100%, and the conversion rate of pentafluoropropionyl fluoride was 100%. The selectivity is 99.8%.

[0051] After rectification, high-purity pentafluoropropionyl fluoride was isolated, and the boiling point of pentafluoropropionyl fluoride was -26.5°C (pressure 760mmHg).

Embodiment 3

[0053] Fill 10 milliliters of the addition catalyst 10%CsF / 90%CrF that the above-mentioned method prepares in the tubular reactor made of Incon alloy of inner diameter 1 / 2 inch, long 30cm 3 . The reaction conditions are as follows: the reaction temperature is raised to 160°C, the molar ratio of carbonyl fluoride to hexafluoropropylene is 1:1, the contact time is 0.25s, and the reaction pressure is 0.1MPa. The reaction product was collected by a sampling bag made of polytetrafluoroethylene. After 10 hours of reaction, a sample was taken from the sampling bag for GC analysis. The reaction result was: the conversion rate of hexafluoropropylene was 97.4%, and the selection of heptafluoroisobutyryl fluoride was 97.4%. The sex is 98.8%.

[0054] After rectification, high-purity heptafluoroisobutyryl fluoride is separated and obtained, and the boiling point of heptafluoroisobutyryl fluoride is -2~4°C (pressure is 760mmHg).

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Abstract

The invention discloses a method for preparing pentafluoride ethyl perfluoro isopropyl ketone through gas phases. The method is characterized in that under the existence of addition catalysts, hexafluoropropylene and hexafluoropropylene oxide or pentafluoropropionyl fluoride take gas phase addition reaction to obtain the pentafluoride ethyl perfluoro isopropyl ketone, or tetrafluoroethylene and heptafluorobutyl fluoride take gas phase addition reaction to obtain the pentafluoride ethyl perfluoro isopropyl ketone. The method has the advantages that the reaction route is short; in addition, rawmaterials such as the hexafluoropropylene, the tetrafluoroethylene, the hexafluoropropylene oxide and carbonyl fluoride can be easily obtained; the cost is low; the yield of the pentafluoride ethyl perfluoro isopropyl ketone is high; the continuous large-scale industrial production can be realized through the route.

Description

technical field [0001] The invention relates to a method for preparing pentafluoroethyl perfluoroisopropyl ketone in gas phase, in particular to a gas phase addition reaction of hexafluoropropylene and hexafluoropropylene oxide or pentafluoropropionyl fluoride in the presence of a catalyst, Or tetrafluoroethylene and heptafluoroisobutyryl fluoride undergo gas phase addition reaction to obtain pentafluoroethyl perfluoroisopropyl ketone. Background technique [0002] Up to now, various documents have disclosed four routes for the synthesis of pentafluoroethyl perfluoroisopropyl ketone. [0003] The first route is the isomerization route. The literature [Journal of Organic Chemistry USSR (English Translation), 1986, 22: 80-85] reported that in ethylene glycol dimethyl ether solvent, 50 ° C, cesium fluoride catalyzed 2,3-difluoro-2-(perfluoro Propan-2-base)-3-(trifluoromethyl)oxirane obtains the pentafluoroethyl perfluoroisopropyl ketone that productive rate is 92%, and equati...

Claims

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Application Information

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IPC IPC(8): C07C45/58C07C45/69C07C49/167
CPCC07C45/58C07C45/69C07C51/58C07C49/167C07C53/50
Inventor 张呈平郭占英马晓迅权恒道
Owner 泉州宇极新材料科技有限公司
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