Method and device for preparing heptafluoroisobutyronitrile

A technology for heptafluoroisobutyronitrile and methyl heptafluoroisobutyrate, which is applied in the field of devices for synthesizing heptafluoroisobutyronitrile, can solve the problems of difficult operation, complicated equipment, long process and the like, achieves simplified operation process, reduced The effect of equipment investment

Pending Publication Date: 2020-05-29
昊华气体有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

During the process, materials need to be transferred and multi-step operations such as washing, extraction, liquid separation, and drying are used. The process is long, the equipment is complicated, and the operation is difficult.

Method used

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  • Method and device for preparing heptafluoroisobutyronitrile

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Embodiment 1

[0017] Such as figure 1 Shown, a kind of synthesis device of heptafluoroisobutyronitrile comprises high and low temperature cycle machine 1, reaction kettle 2, condenser 3, solvent recovery tank 4, freezing collection tank 5, liquid delivery pump 6, sight glass 7, vacuum system 8. The high and low temperature cycle machine is connected to the jacket of the reaction kettle, the liquid delivery pump 6 is connected to the top of the reaction kettle, the outlet on the top of the reaction kettle is respectively connected to the condenser 3 and the solvent recovery tank 4 through a tee, and the tee and the solvent recovery tank 4 are installed There is a tube-type sight glass 7; the outlet of the condenser 3 is connected to the frozen collection tank 5 and the vacuum system 8 through another tee. There is a vent on the top to connect with the atmosphere to balance the pressure in the solvent collection tank during operation. The device also includes an electric circuit, and the el...

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PUM

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Abstract

The invention discloses a method and device for preparing heptafluoroisobutyronitrile, wherein the method comprises the steps: adding methyl heptafluoroisobutyrate into a reaction kettle, adding an alcoholic solution of ammonia, and controlling the reaction temperature to be lower than 0 DEG C; carrying out a reaction for 2-5 h, heating to 60 DEG C, finishing the reaction when the content of methyl heptafluoroisobutyrate in a reaction solution is less than 0.1%, removing a methanol solvent by vacuum distillation, and removing the vacuum when the content of methanol in the reaction solution inthe reaction kettle is less than 1%; and adding a dimethylformamide/pyridine solvent into the reaction system, controlling the reaction temperature to be lower than 0 DEG C, adding a dehydrating agenttrifluoroacetic anhydride, and collecting heptafluoroisobutyronitrile gas. According to the method, an intermediate heptafluoroisobutyrylamide synthesis step and a step device for preparing heptafluoroisobutyronitrile by dehydrating heptafluoroisobutyrylamide are integrated; transfer of an intermediate heptafluoroisobutyramide is not needed and water washing, extraction, recrystallization and other operations are avoided, so the heptafluoroisobutyronitrile is directly synthesized, the equipment investment is greatly reduced, the operation process is simplified, and the method is suitable forindustrial production.

Description

technical field [0001] The invention relates to a synthesis device of heptafluoroisobutyronitrile, in particular to a device for synthesizing heptafluoroisobutyronitrile through ammoniation and dehydration of heptafluoroisobutyronitrile. Background technique [0002] Heptafluoroisobutyronitrile is a new type of environmentally friendly insulating gas material. It has the characteristics of low boiling point, high volatility, excellent electrical insulation properties and good environmental performance. It can be used as a dielectric composition for electrical equipment insulators. The greenhouse effect index (GWP) of heptafluoroisobutyronitrile is only 2210, which is much lower than that of sulfur hexafluoride (GWP=23500). It can be used to replace the traditional sulfur hexafluoride insulating gas and greatly reduce the problem of atmospheric greenhouse effect. Heptafluoroisobutyronitrile has received widespread attention from the global electrical industry and has begun to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C255/10C07C231/02C07C233/05
CPCC07C253/20C07C231/02C07C233/05C07C255/10
Inventor 任章顺牛鹏飞袁胜芳李前进张金彪
Owner 昊华气体有限公司
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