Preparation method for pentafluoroethyl trifluoromethyl ether

A technology of pentafluoroethyl trifluoromethyl ether and trifluoromethyl hypofluorite, which is applied in the field of preparation of fluorine-containing ether compounds, and can solve the problems of harsh reaction conditions and only 10-20% of perfluorinated organic compounds , to achieve the effect of increasing the yield

Inactive Publication Date: 2018-04-03
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, when using the electrochemical fluorination method to synthesize, it must have a certain solubility in anhydrous hydrogen fluoride, and the yield of this synthesis method is generally not too high. In enterprises, the yield of perfluorinated organic compounds is generally only 10-20%.
The cobalt trifluoride method is because of its harsh reaction conditions, and there is no report on the use of this method for industrial production in China.

Method used

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  • Preparation method for pentafluoroethyl trifluoromethyl ether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] For the structure of the equipment for the reaction, see figure 1 , the material of the reaction kettle main body 1 is 304 stainless steel, and it is provided with a refrigerated medium jacket 2, a pressure monitoring point and a temperature monitoring device 3, and the temperature sensing part of the temperature monitoring device 3 extends below the liquid surface of the solvent; the tetrafluoroethylene feed pipe 4 and trifluoromethyl hypofluorite feed pipe 5 all lead to the bottom of the reactor, and the two feed pipes are on different sides. An anchor stirrer 6 is arranged in the reactor.

[0029] Inject 1.2L of liquid perfluoro-n-pentane into the reactor (capacity is 2L) at room temperature, then start the low-temperature circulation pump to pass the frozen alcohol into the jacket of the reactor, gradually cool down the reactor, and start the reactor The stirrer, the rotating speed is adjusted to 200r / min, and then the flow rate of 10L / h is blown into the reaction ...

Embodiment 2

[0032] Reaction equipment is with embodiment 1.

[0033] Inject 1.2L of liquid perfluoro-n-pentane into the reaction kettle at room temperature, then start the low-temperature circulation pump to pass the frozen alcohol into the freezing medium jacket of the reaction kettle, gradually cool down the reaction kettle, and start the agitator of the reaction kettle , the rotating speed is adjusted to 200r / min, and then the flow rate of 10L / h is blown into the reactor to replace with refined nitrogen (purity 99.99%, moisture content less than 20ppm), and after the temperature in the reactor drops to -85°C and stabilizes, Nitrogen was stopped, and tetrafluoroethylene (CF 2 = CF 2), after 20 minutes, trifluoromethyl hypofluorite (CF 3 OF) to react, the reaction tail gas is condensed and refluxed by the condenser, washed with 20% KOH lye, and then emptied, the reaction temperature is maintained at -82 ± 5 ° C, and the reaction is carried out at normal pressure for 2 hours. Stop feedi...

Embodiment 3

[0036] The reaction conditions were as in Example 1, the reaction solvent was replaced with dichloromethane, and the amount added was also 1.2 L. Other conditions remained unchanged. After the reaction, the purity of 98% pentafluoroethyltrifluoromethyl was obtained. 298 g of ether, the yield of pentafluoroethyl trifluoromethyl ether was 64.2%.

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Abstract

The invention belongs to the field of organic compounds, and provides a preparation method for pentafluoroethyl trifluoromethyl ether. The preparation method comprises the following steps: with trifluoromethyl hypofluoride and tetrafluoroethylene as raw materials, adding the trifluoromethyl hypofluoride and the tetrafluoroethylene into a reaction device with the presence of a solvent, carrying outa reaction under conditions of protection of gas and a temperature of minus 90 to minus 30 DEG C so as to synthesize a crude pentafluoroethyl trifluoromethyl ether product, and subjecting the crude pentafluoroethyl trifluoromethyl ether product to rectification and purification so as to obtain the pentafluoroethyl trifluoromethyl ether with high purity. The invention provides a reliable chemicalmethod to synthesize the pentafluoroethyl trifluoromethyl ether; the trifluoromethyl hypofluoride and the tetrafluoroethylene are used as the raw materials; a free-radical addition reaction is generated; expensive catalysts are not needed; a reaction under industrial scale can be realized; and the yield is improved through strict control of reaction conditions.

Description

technical field [0001] The invention belongs to the field of organic compounds, and in particular relates to a preparation method of fluorine-containing ether compounds. Background technique [0002] Perfluoroalkyl ether refers to an ether formed by replacing all the hydrogen atoms on the carbon atoms in the alkyl ether molecule with fluorine atoms. This type of compound has special properties such as strong acid resistance, strong alkali resistance, and high chemical stability. It is Non-conductive, colorless, odorless, non-toxic, non-flammable, basically non-toxic, and not easy to decompose when heated, it can be used in biology, medicine, chemical engineering, electronics, military industry and other fields. [0003] Among the perfluoroalkyl ethers, pentafluoroethyl trifluoromethyl ether is widely used as refrigerant, cleaning agent and abrasive for electronic components, dielectric medium of gas, new fire extinguishing agent, Circulating working fluid of thermal power s...

Claims

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Application Information

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IPC IPC(8): C07C41/06C07C43/12
CPCC07C41/06C07C43/123
Inventor 庹洪刘波吕太勇罗源军李俊玲宋亦兰
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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