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Method for preparing perfluoroisobutyronitrile from hexafluoropropylene dipolymer as well as perfluoroisobutyronitrile and application

A technology of hexafluoropropylene dimerization and hexafluoropropylene dimer is applied in perfluoroisobutyronitrile and application fields, and can solve the problem of high equipment cost, unfavorable industrial scale-up production, high cost of electrolytic electrode plate production, and isobutyric anhydride raw material. It is not easy to obtain and other problems, and achieves the effects of low global warming effect, high yield and short reaction route.

Inactive Publication Date: 2019-03-22
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 preparing perfluoroisobutyronitrile from hexafluoropropylene dipolymer as well as perfluoroisobutyronitrile and application
  • Method for preparing perfluoroisobutyronitrile from hexafluoropropylene dipolymer as well as perfluoroisobutyronitrile and application
  • Method for preparing perfluoroisobutyronitrile from hexafluoropropylene dipolymer as well as perfluoroisobutyronitrile and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Preparation of hexafluoropropylene dimer raw materials: hexafluoropropylene gas was passed through a catalytic reaction tube equipped with NaF / Al2O3 catalyst, the catalyst loading was 10%, the contact time was 0.1s; the temperature of the catalytic reaction tube At 150°C, the reacted mixed gas enters the condenser with a cooling jacket from the gas port inlet, the temperature of the condensed water is 10°C, and the unreacted hexafluoropropylene is circulated to the catalytic reaction tube through the gas outlet. The purity of the liquid hexafluoropropylene dimer in the receiver of the condenser was detected to be 99.3%. The yield of hexafluoropropylene dimer is shown in Table 1.

Embodiment 2

[0026] Example 2: Preparation of hexafluoropropylene dimer raw materials: hexafluoropropylene gas was passed through a catalytic reaction tube equipped with AgF / C catalyst, the catalyst loading was 15%, the temperature of the catalyst packing column was 180°C, and the contact time It is 10s. The reacted mixed gas enters the condenser with cooling jacket from the air inlet, and the temperature of the condensed water is 10°C; the unreacted hexafluoropropylene is circulated to the catalytic reaction column through the outlet. The purity of the liquid hexafluoropropylene dimer in the condenser is 99.2%. The yield of hexafluoropropylene dimer after application is shown in Table 1.

Embodiment 3

[0027] Example 3: Preparation of hexafluoropropylene dimer raw materials: hexafluoropropylene gas was passed through a catalytic reaction tube equipped with KF / C catalyst, the catalyst loading was 20%, the temperature of the catalyst packing column was 220°C, and the contact time It is 30s; the reacted mixed gas enters the condenser with 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 through the outlet. The purity of the liquid hexafluoropropylene dimer in the condenser was detected to be 99.3%. The yield of hexafluoropropylene dimer after application is shown in Table 1.

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Abstract

The invention belongs to the field of fluorine chemical industry and specifically relates to a method for preparing perfluoroisobutyronitrile from hexafluoropropylene dipolymer as well as perfluoroisobutyronitrile and application. The preparation method comprises the following steps: 1) sending the hexafluoropropylene dipolymer into an oxidizing furnace to perform cracking reaction with oxygen under the catalyst condition; separating to obtain perfluoro isobutyryl fluoride; 2) performing continuous amination reaction and dehydration reaction on the perfluoro isobutyryl fluoride under an amination reagent and a dehydration reagent existence condition to obtain the perfluoroisobutyronitrile. The method disclosed by the invention can be performed in an intermittent mode or a continuous mode,the conditions are controllable, a reaction route is short, a yield is high, a product is easy to separate, and the method is suitable for industrial amplification production.

Description

Technical field [0001] The invention belongs to the field of fluorine chemicals, and specifically relates to a method for preparing perfluoroisobutyronitrile from a hexafluoropropylene dimer, and perfluoroisobutyronitrile and applications. Background technique [0002] Perfluoroisobutyronitrile has the characteristics of low boiling point, high volatility, excellent electrical insulation properties and good environmental performance. It can be used as a gas dielectric material and used as a dielectric composition for insulators in electrical devices. The greenhouse effect index (GWP) of perfluoroisobutyronitrile is only 2100, which is much lower than sulfur hexafluoride (GWP=23500). It can be used to replace 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 used. [0003] High-quality perfluoroisobutyryl f...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/10C07C51/58C07C53/50C07C231/02C07C233/05H01B17/56
CPCC07C51/58C07C231/02C07C253/20C07C255/10H01B17/56C07C53/50C07C233/05
Inventor 汤峤永姚素梅贺光瑞李希仑
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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