Method of preparing pentafluoroethyl isopropyl ketone

A technology of perfluoroethyl isopropyl ketone and hexafluoropropylene, which is applied in the field of preparation of perfluoroethyl isopropyl ketone, can solve the problems of low selectivity, difficult manipulation, and many by-products, and achieve a high degree of automation , easy operation and low equipment requirements

Active Publication Date: 2017-01-11
航天康达(北京)科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] 5. Reaction of perfluoropropylene oxide and hexafluoropropylene: This route (as follows) reacts perfluoropropylene oxide and hexafluoropropylene at 20-25°C under the catalysis of cesium fluoride to prepare perfluorohexanone (Zh.Vses , Khim, 0-va, 1978,23(2), 236-237(Russ)), the advantage of this route is exactly that condition is gentle, and raw material is

Method used

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  • Method of preparing pentafluoroethyl isopropyl ketone
  • Method of preparing pentafluoroethyl isopropyl ketone
  • Method of preparing pentafluoroethyl isopropyl ketone

Examples

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Embodiment 1

[0060] A method for preparing perfluoroethyl isopropyl ketone, comprising the steps:

[0061] (1) Mix 540L 1,1,2-trichlorotrifluoroethane (Freon 113), 300L sodium hypochlorite aqueous solution (active chlorine content 10%), 2Kg tetrabutylammonium chloride and 2Kg perfluoroalkyl polyether (FN -6810) into a 1000L autoclave with stirring (type 316 stainless steel). The reaction system was cooled to minus 10°C, the air in the reaction kettle was evacuated, 260Kg of hexafluoropropylene (measured by weight loss method) was introduced, the temperature was controlled at -10°C to -5°C, and the reaction was performed for 2 hours. After the reaction was stopped, let stand for 15 minutes. , Sampling detection, gas chromatography results show that the conversion rate of hexafluoropropylene is 97%, and the yield of hexafluoropropylene oxide is 93%. The organic phase (1,1,2-trichlorotrifluoroethane) was transferred to another reaction kettle from the lower discharge port of the reaction ket...

Embodiment 2

[0064] A method for preparing perfluoroethyl isopropyl ketone, the preparation method is the same as that in Example 1, the difference is only that: the phase transfer catalyst tetrabutylammonium chloride in step (1) is replaced with trioctyl methyl chloride ammonium chloride, and the solvent in step (2), dimethyl ether oxalate, was replaced with acetonitrile.

[0065] After testing, after the reaction in step (1), the conversion rate of hexafluoropropylene was 99%, and the yield of hexafluoropropylene oxide was 94%; after the reaction in step (2), the conversion rate of hexafluoropropylene was 100%, The yield of perfluorohexanone is 72%, the main impurity is hexafluoropropylene dimer

[0066] (22.3%).

Embodiment 3

[0068] This example is the same as Example 1, the difference is only that the solvent in step (2) is replaced with N,N-dimethylformamide. After the reaction in step (2), the conversion rate of hexafluoropropylene was 100%, the yield of perfluorohexanone was 76%, and the main impurity was hexafluoropropylene dimer (18.3%).

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Abstract

The invention relates to the technical field of organic synthesis, in particular to a method of preparing pentafluoroethyl isopropyl ketone. The method includes the steps that hexafluoropropylene oxide and hexafluoropropylene are used as raw materials and react at the temperature of 65-80 DEG C in the presence of a crown ether phase transfer catalyst and fluorine-containing salt to obtain pentafluoroethyl isopropyl ketone. The yield of the product prepared through the method is 88-91%, and the conversion rate of the raw material hexafluoropropylene is up to 100%. The method has the advantages of being easy to operate, low in requirement for equipment, low in cost, high in automation degree and high in equipment use ratio and can meet the requirement for industrial production application.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing perfluoroethyl isopropyl ketone. Background technique [0002] Perfluoroethyl isopropyl ketone is referred to as perfluorohexanone (the structure is as follows), and the full chemical name is 1,1,1,2,2,4,5,5,5-nonafluoro-4-trifluoromethyl- Pent-3-one, English name (1,1,1,2,2,4,5,5,5-nonofluoro-4-trifluoromethyl-pentane-3-one), chemical formula CF 3 CF 2 COCF(CF 3 ) 2 , ASHRAE chemical code FK-5-1-12. Perfluorohexanone was synthesized by scientists from the former Soviet Union as a fine chemical intermediate as early as the 1970s, but it has not been produced and applied on a large scale. Until 2001, 3M company launched a trade name NOVEC 1230 TM The high-efficiency fluoroalkane fire extinguishing agent is used to replace the environmentally unfriendly chlorofluorocarbons (perchlorofluorocarbons) and halons (bromofluoroalkanes), and perfluoro...

Claims

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Application Information

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IPC IPC(8): C07C45/58C07C49/167
CPCC07C45/58C07C49/167
Inventor 苗广州
Owner 航天康达(北京)科技发展有限公司
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