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Method for generating perfluoroisobutyronitrile by cracking of hexafluoropropylene trimer, perfluoroisobutyronitrile and application for perfluoroisobutyronitrile

A technology of hexafluoropropylene trimer and perfluoroisobutyronitrile, applied in chemical instruments and methods, preparation of organic compounds, dehydration preparation of carboxylic acid amides, etc., can solve the disadvantages of difficult separation, low electrolysis efficiency, and high equipment cost Problems such as industrial scale-up production, to achieve the effect of short reaction route

Inactive Publication Date: 2019-04-12
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] High-quality perfluoroisobutyryl fluoride is an important intermediate for the preparation of perfluoroisobutyryl nitrile. At present, the preparation method of perfluoroisobutyryl fluoride is the electrochemical fluorination of isobutyric anhydride (in U.S. Patent No.2713593 and R.E. There are methods in Banks, Preparation, Properties and Industrial Applications of Organofluorine Compounds, pages 19-43, Halsted Press, New York (1982), but the raw material of isobutyric anhydride is not easy to get
In the US6013795A electrolytic synthesis method, the raw materials are relatively cheap, but what is obtained is a mixture of isobutyryl fluoride and n-butyryl fluoride, which is difficult to separate
In addition, the electrolysis efficiency is low, the production cost of the electrolysis plate is expensive, and the high equipment cost is not conducive to industrial scale-up production

Method used

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  • Method for generating perfluoroisobutyronitrile by cracking of hexafluoropropylene trimer, perfluoroisobutyronitrile and application for perfluoroisobutyronitrile
  • Method for generating perfluoroisobutyronitrile by cracking of hexafluoropropylene trimer, perfluoroisobutyronitrile and application for perfluoroisobutyronitrile
  • Method for generating perfluoroisobutyronitrile by cracking of hexafluoropropylene trimer, perfluoroisobutyronitrile and application for perfluoroisobutyronitrile

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Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: Preparation of hexafluoropropylene trimer raw material: Hexafluoropropylene gas is passed through the catalytic reaction tube equipped with NaF / Al2O3 catalyst, the loading capacity of the catalyst is 10%, the temperature of the catalytic reaction tube of the catalyst is 260 ℃, contact The time is 0.1s; the reacted mixed gas enters the condenser with a cooling jacket from the air inlet, the temperature of the condensed water is 10°C, and the unreacted hexafluoropropylene is circulated to the catalytic reaction tube of the catalyst through the outlet. The purity of the liquid hexafluoropropylene trimer in the condenser was detected to be 99.3%. The yield of hexafluoropropylene trimer is shown in Table 1.

Embodiment 2

[0028] Example 2: Preparation of raw materials for hexafluoropropylene trimer: pass hexafluoropropylene gas through a catalytic reaction tube equipped with an AgF / C catalyst, the loading of the catalyst is 15%, the temperature of the catalytic reaction tube of the catalyst is 300 ° C, contact The time is 10s; the reacted mixed gas enters the condenser with a cooling jacket from the air inlet, the temperature of the condensed water is 10°C, and the unreacted hexafluoropropylene is circulated to the catalytic reaction tube of the catalyst through the outlet. The purity of the liquid hexafluoropropylene trimer in the condenser was detected to be 99.3%. The productive rate of hexafluoropropylene trimer after applying mechanically is shown in Table 1.

Embodiment 3

[0029] Example 3: Preparation of hexafluoropropylene trimer raw material: Hexafluoropropylene gas is passed through a catalytic reaction tube equipped with a KF / C catalyst, the loading of the catalyst is 20%, and the temperature of the catalytic reaction tube of the catalyst is 320°C. The time is 30s; the reacted mixed gas enters the condenser with a cooling jacket through the air inlet, the temperature of the condensed water is 10°C, and the unreacted hexafluoropropylene is circulated to the catalytic reaction tube of the catalyst through the outlet. The purity of the liquid hexafluoropropylene trimer in the condenser was detected to be 99.3%. The productive rate of hexafluoropropylene trimer after applying mechanically is shown in Table 1.

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Abstract

The invention belongs to the field of fluorine chemistry, and specifically relates to a method for generating perfluoroisobutyronitrile by cracking of a trimer, the perfluoroisobutyronitrile and an application for the perfluoroisobutyronitrile. The preparation method comprises the following steps: 1) allowing a hexafluoropropylene trimer to enter an oxidation furnace for a cracking reaction with oxygen under the condition of a catalyst, and carrying out separation so as to obtain perfluoroisobutyryl fluoride; and 2) continuously subjecting the perfluoroisobutyryl fluoride to an amination reaction and a dehydration reaction in the presence of an amination reagent and a dehydration reagent so as to obtain the perfluoroisobutyronitrile. The method for generating the perfluoroisobutyronitrileby cracking of the hexafluoropropylene trimer provided by the invention has mild reaction conditions and high product yield, is free of pollution and facilitates scale production. Meanwhile, the raw material namely the hexafluoropropylene trimer is controllable in preparation and has high conversion efficiency.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry, and in particular relates to a method for generating perfluoroisobutyronitrile by cracking a trimer, perfluoroisobutyronitrile and its application. Background technique [0002] Perfluoroisobutyronitrile 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 perfluoroisobutyronitrile is only 2100, 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. Perfluoroisobutyronitrile has received widespread attention from the global electrical industry and has begun to be applied. [0003] High-qualit...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/10
CPCC07C45/34C07C253/20C07C255/10C07C49/167
Inventor 贺光瑞姚素梅肖鑫李希仑
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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