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Synthesizing method of fluorine halogenated vinyl ether

A fluorohaloalkene ether and a synthesis method technology are applied in the field of fluorohaloalkene ether synthesis, can solve the problems of difficulty in obtaining perfluoropolyether diacyl fluoride, low product selectivity, harsh reaction conditions and the like, and achieve a technological process Short, high yield, good product quality effect

Inactive Publication Date: 2016-04-20
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the reaction raw material perfluoropolyether diacyl fluoride is difficult to obtain and expensive; the reaction needs to be carried out at a very low temperature, the reaction time is long, the reaction conditions are harsh, and the product selectivity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Put 2 mol of tetrafluoropropanol, 4 mol of DMSO (dimethyl sulfoxide), and 3 mol of NaOH into a 2L stainless steel high-pressure reactor, heat up to 100°C, and continuously feed tetrafluoroethylene under stirring for reaction. The flow rate of the feed keeps the pressure in the reactor at 0.8MPa, and the reaction temperature is controlled by the jacketed refrigerant to 100°C. When the flow rate of tetrafluoroethylene is 0.5% of the initial flow rate, stop feeding tetrafluoroethylene, and rectify and separate Obtain trifluoropropenyltetrafluoroethyl ether (CF 2 = CFCH 2 OCF 2 CF 2 H) 1.828 moles, 99.9% purity, 91.4% yield.

[0029] In a 1000ml four-neck flask with mechanical stirring and a reflux condenser, add the trifluoropropenyltetrafluoroethyl ether (CF) obtained in the previous step. 2 = CFCH 2 OCF 2 CF 2 H) 1.828mol, and bromine 2.376mol, stirring, under light, 45 ° C reaction for 2h, the reaction solution was washed with alkali and separated to obtain dibro...

Embodiment 2

[0032] Put 2 mol of tetrafluoropropanol, 3 mol of DMF (N,N-dimethylformamide) and 2.4 mol of KOH into a 2L stainless steel autoclave, raise the temperature to 90°C, and continuously feed ethylene under stirring for reaction. Adjust the flow rate of ethylene to keep the pressure in the reactor at 1.0MPa, control the reaction temperature to 90°C through the jacketed refrigerant, stop feeding ethylene when the flow rate of ethylene is 0.6% of the initial flow rate, and rectify the reaction liquid Trifluoropropenyl ethyl ether (CF 2 = CFCH 2 OCH 2 CH 3 ) 1.74mol, the purity is 99.8%, and the yield is 87.0%.

[0033] In a 1000ml four-necked flask with mechanical stirring and a reflux condenser, add the trifluoropropenyl ethyl ether (CF 2 = CFCH 2 OCH 2 CH 3 ) 1.74mol, and iodine 2.088mol, stirred and reacted at 30°C for 1.5h under light, and the reaction solution was washed with alkali and separated to obtain diiodotrifluoropropyl ethyl ether (CF 2 ICFICH 2OCH 2 CH 3 ) 1...

Embodiment 3

[0036] Put 2 mol of trifluorobutanol, 5 mol of DMF (N,N-dimethylformamide) and 4 mol of sodium ethoxide into a 2L stainless steel autoclave, heat up to 150°C, and continuously feed vinylidene fluoride under stirring for reaction. The reaction process In the process, the pressure in the reactor is kept at 0.5 MPa by adjusting the flow rate of vinylidene fluoride, and the reaction temperature is controlled by jacket refrigerant to 150°C. When the flow rate of vinylidene fluoride is 0.7% of the initial flow rate, the flow of vinylidene fluoride is stopped Vinyl fluoride, the reaction solution is rectified and separated to obtain difluorobutenyl difluoroethyl ether (CF 2 =CHCH 2 CH 2 OCF 2 CH 3 ) 1.696mol, the purity is 99.5%, and the yield is 84.8%.

[0037] In a 1000ml four-necked flask with mechanical stirring and a reflux condenser, add the difluorobutenyl difluoroethyl ether (CF 2 =CHCH 2 CH 2 OCF 2 CH 3 ) 1.696mol, and bromine 2.544mol, stirring, under light, 50 ℃ r...

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Abstract

The invention discloses a synthesizing method of fluorine halogenated vinyl ether. The method includes the steps of firstly, adding alcohol, solvent and a catalyst into a reaction still, continuously introducing olefin for reaction, controlling the pressure of the reaction still by adjusting the introduction amount of olefin in the reaction process, stopping the introduction of olefin when the introduction flow of olefin is 0.5-1.5% of the initial introduction flow, and fine distilling reaction liquid to obtain fluorine-containing vinyl ether, wherein at least one of alcohol and olefin contains fluorine; secondly, making fluorine-containing vinyl ether and elemental halide react under illumination, and conducting alkaline washing and liquid separating on reaction liquid to obtain fluorine halogenated ether; thirdly, adding fluorine halogenated ether to a triethylamine solution of sodium alkoxide to react, and conducting liquid separating and fine distilling on reaction liquid to obtain fluorine halogenated vinyl ether. The method has the advantages that raw materials are easy to obtain, reaction conditions are mild and yield is high.

Description

technical field [0001] The invention relates to the technical field of fluorine fine chemical industry, in particular to a synthesis method of fluorohaloalkene ether. Background technique [0002] Fluorohalogenated alkenyl ethers, especially fluorohalogenated alkenyl ethers whose end groups are substituted by halogen atoms, not only have end groups and double bond active groups, but also have the advantages of low surface tension and high stability of fluorine-containing chemicals. It plays an important role in organic synthesis, and is an important medicine, pesticide intermediate and substitute for Freon compounds. Fluorohalogenated alkenyl ethers whose terminal groups are substituted by halogen atoms also have important uses in the synthesis of organic chemicals and medicines, and their synthesis methods are currently the focus of research. [0003] For example, Chinese Patent Publication No. CN1660740A, date of publication August 31, 2005, title of invention: method for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/17C07C41/24
CPCC07C41/06C07C41/22C07C41/24
Inventor 耿为利周强王宗令吴庆王树华张文革
Owner JUHUA GROUP TECH CENT
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