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Preparation method of perfluoronitrile type compound

A compound and perfluoronitrile technology, applied in the field of preparation of perfluoronitrile compounds, can solve the problems of low yield and uneconomical perfluoronitrile compounds, and achieve the effects of easy availability of raw materials, simple operation and high yield

Active Publication Date: 2018-11-23
GUANGDONG POWER GRID CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a method for preparing perfluoronitrile compounds, which solves the low yield and uneconomical technical problems of existing perfluoronitrile compounds

Method used

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  • Preparation method of perfluoronitrile type compound

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Embodiment 1

[0038] Under the protection of nitrogen replacement, 12.76g (0.22mol) of potassium fluoride, 12.29g (0.20mol) of cyanogen chloride, and 100mL of acetonitrile were added to a 500mL dry autoclave, and 33.00g ( 0.22mol), 50 ℃ airtight reaction for 10 hours. After the reaction is completed, the reaction solution is volatilized at 5°C in an alcohol low-temperature cooling tank, and the volatile components are collected at -40°C. The product perfluoroisobutyronitrile at -5°C was 27.60 g, and the yield was 70.4%.

Embodiment 2

[0040] Under the protection of nitrogen replacement, 9.24g (0.22mol) of sodium fluoride, 12.29g (0.20mol) of cyanogen chloride, and 100mL of acetonitrile were added to a 500mL dry autoclave, and 33.00g ( 0.22mol), 50 ℃ airtight reaction for 10 hours. After the reaction is completed, the reaction liquid is volatilized at 5°C in an alcohol low-temperature cooling tank, and the volatile components are collected at -40°C, and the volatile components are volatilized at -20°C to remove unreacted hexafluoropropylene, and then volatilized and collected to obtain the boiling point It was 27.51 g of perfluoroisobutyronitrile at -5°C, and the yield was 70.2%.

Embodiment 3

[0042] Under the protection of nitrogen replacement, add 12.76g (0.22mol) of potassium fluoride (0.22mol), 12.29g (0.20mol) of cyanogen chloride, and 100mL of diethylene glycol dimethyl ether into a 500mL dry autoclave. 33.00 g (0.22 mol) of perfluoropropene was reacted at 50° C. for 10 hours in a sealed manner. After the reaction is completed, the reaction solution is volatilized at 5°C in an alcohol low-temperature cooling tank, and the volatile components are collected at -40°C, and the volatile components are volatilized at -20°C to remove unreacted hexafluoropropylene, and then evaporated and collected to obtain the boiling point It was 25.60 g of perfluoroisobutyronitrile at -5°C, and the yield was 65.3%.

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Abstract

The invention relates to the technical field of organic synthesis and in particular relates to a preparation method of a perfluoronitrile type compound. The invention discloses the preparation methodof the perfluoronitrile type compound; the preparation method comprises the following step: taking a perfluoroalkene type compound, metal fluoride and cyanogen chloride to react under nitrogen gas orinert gas displacement and protection, so as to obtain the perfluoronitrile type compound. The preparation method adopts a one-pot method to synthesize the perfluoronitrile type compound and is simpleto operate; a byproduct of the reaction is sodium chloride or potassium chloride and has no pollution to the environment; post-treatment is easy to operate. Furthermore, the perfluoronitrile type compound prepared by the preparation method has high yield and the highest yield is 82.1 percent; the perfluoronitrile type compound has high purity and the purity is higher than 99.3 percent; the technical problems that an existing perfluoronitrile type compound has relatively low yield and is uneconomical are solved.

Description

technical field [0001] The present invention relates to the technical field of organic synthesis, in particular to a preparation method of perfluoronitrile compounds. Background technique [0002] GIS (gas-insulated switchgear) is the English abbreviation of gas-insulated fully enclosed switchgear, which is widely used in the high-voltage electrical field. SF 6 Gas is widely used in GIS because of its excellent insulation and arc extinguishing properties. However, SF 6 The global warming potential value (Global Warming Potential, GWP) is about 22800 (with 100 years as the evaluation time of global warming potential, CO 2 Tignor, S.K.; Allen, J.; Boschung, A.; et al. IPCC, 2013; Climate Change 2013: The Physical Science Basis .Contribution of Working Group I to the FifthAssessment Report of the Intergovernmental Panel on Climate Change; Cambridge University Press: Cambridge, United Kingdom and New York, NY, USA, 2013), so it is listed as one of the six requirements in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/30
CPCC07C253/30C07C255/03
Inventor 李丽吴永明樊小鹏田长青周永言唐念邹庄磊
Owner GUANGDONG POWER GRID CO LTD
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