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Synthesis method of heptafluoroisobutyronitrile

A technology of heptafluoroisobutyronitrile and synthesis method, which is applied in the field of synthesis of heptafluoroisobutyronitrile, can solve problems such as environmental pollution, increased production cost, and long route, and achieve simple and safe process operation, reaction conversion rate and yield High, the effect of high product purity

Inactive Publication Date: 2020-10-16
福建省漳平市九鼎氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this technical route is mature and reliable, there is a long route, and the involved chemicals such as dehydrating agents lead to increased production costs and environmental pollution issues related to emissions, etc.

Method used

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  • Synthesis method of heptafluoroisobutyronitrile
  • Synthesis method of heptafluoroisobutyronitrile
  • Synthesis method of heptafluoroisobutyronitrile

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Embodiment 1

[0086] A kind of synthetic method of heptafluoroisobutyronitrile of the present invention, its synthetic route figure is as figure 1 shown. This synthetic method comprises the following steps:

[0087] Step (1): Synthesis of Heptafluoroisobutyrate

[0088] First, the reaction system is heated and vacuumized to remove water, and the whole system is purged with high-purity nitrogen to remove oxygen therein; the reactor is cooled to normal temperature, and under the protection of nitrogen, tetraethylene glycol dimethyl ether (222.28g, 1mol), dry cesium fluoride (89.6g, 0.59mol), stirred, heated to 70°C; then metered into hexafluoropropylene (HFP) (118.5g, 0.79mol) and carbon dioxide (44g, 1.00mol) , During the process, the pressure of the reactor is controlled at 0.1Mpa to 0.5Mpa, and the reaction is kept for 8 hours. After the reaction, separate the fluorocarbon layer (HFP dimer / trimer, about 21g), filter the TG layer (tetraethylene glycol dimethyl ether) to remove TG, wash t...

Embodiment 2

[0097] A kind of synthetic method of heptafluoroisobutyronitrile of the present invention, its synthetic route figure is as image 3 shown. This synthetic method comprises the following steps:

[0098] Step (1): Synthesis of Heptafluoroisobutyrate

[0099] First, the reaction system is heated and vacuumized to remove water, and the whole system is purged with high-purity nitrogen to remove oxygen therein; the reactor is cooled to normal temperature, and under nitrogen protection, tetraethylene glycol dimethyl ether (222.28g , 1mol), add dry cesium fluoride (90g, 0.59mol), stir, heat up to 70 ℃; ), the pressure of the reactor was controlled at 0.1MPa~0.2Mpa during the process, and the reaction was kept for 8 hours. After the reaction, separate the fluorocarbon layer (HFP dimer / trimer, about 21g), filter the TG layer (tetraethylene glycol dimethyl ether) to remove TG, wash the filter cake with benzene, and dry the filter cake to obtain heptafluoroisobutyl cesium base salt (1...

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Abstract

The invention discloses a synthesis method of heptafluoroisobutyronitrile, which comprises the following steps: (1) reacting hexafluoropropylene with carbon dioxide under the catalysis of fluoride salt to obtain heptafluoroisobutyrate; (2) acidifying the obtained heptafluoroisobutyric acid, and then carrying out esterification reaction with alcohol to obtain heptafluoroisobutyrate; and (3) reacting the obtained heptafluoroisobutyrate with ammonia, and dehydrating to obtain heptafluoroisobutyronitrile. The synthesis method has the advantages of easily available raw materials, mild reaction conditions, high reaction conversion rate and yield, easy separation and purification, simple and safe process operation, short synthesis route and low cost.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthetic method of heptafluoroisobutyronitrile. Background technique [0002] Heptafluoroisobutyronitrile (perfluoroisobutyronitrile), namely 2,3,3,3-tetrafluoro-2-trifluoromethylpropionitrile, is a class of perfluoronitrile compounds with a boiling point of -4.7°C. It is a colorless gas at normal temperature and pressure. It has the characteristics of low boiling point, high volatility, excellent electrical insulation properties and good environmental protection performance, and can be used as a gas dielectric material and a dielectric composition for insulators in electrical devices. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C51/15C07C51/02C07C53/21C07C67/08C07C69/63C07C253/22C07C255/10
CPCC07C51/02C07C51/15C07C51/412C07C67/08C07C253/22C07C53/21C07C69/63C07C255/10
Inventor 周济苍喻强廖敏周遇吉喻鼎辉
Owner 福建省漳平市九鼎氟化工有限公司
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