Process and device for preparing environmentally-friendly insulating gas perfluoroalkylnitrile

Patent metadata

Field	Value
Publication number	US-10738003-B2
Application number	US-201816616670-A
Country	US
Kind code	B2
Filing date	Jan 12, 2018
Priority date	May 24, 2017
Publication date	Aug 11, 2020
Grant date	Aug 11, 2020

Abstract

Provided are a process and a device for preparing environmentally-friendly insulating gas perfluoroalkylnitrile. The device comprises a first tank reactor, a second tank reactor, and a fixed bed reactor. A condensing and collecting device is provided at the top of the first tank reactor, a collecting and guiding channel at the bottom of the condensing and collecting device is connected to an inlet of a storage tank, and an outlet of the storage tank is connected to an inlet of the second tank reactor. The second tank reactor is connected to a perfluoroolefin tank. An outlet of the second tank reactor is connected to a storage gasification tank. The storage gasification tank is connected to a carrier gas tank, and an outlet of the storage gasification tank is connected to an inlet of the fixed bed reactor. The present invention starts from cyanuric chloride and perfluoropropylene, and uses two tank reactors and a fixed bed reactor to realize production with high atom economy. The preparation method has simple reaction conditions, high atom economy, low cost, and is continuous and enables scale production.

First claim

What is claimed is:

1. A process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile, characterized by comprising: cyanuric chloride and sodium fluoride are subjected to fluorination reaction to generate cyanuric fluoride, then the cyanuric fluoride and perfluoroolefin are subjected to catalytic addition to generate trisperfluoroalkyl triazine, and the trisperfluoroalkyl triazine is carried into a fixed bed reactor by a carrier gas for high-temperature catalytic cracking to obtain the perfluoroalkyl nitrile.

2. The process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile according to claim 1 , characterized in that the fluorination reaction occurs in sulfolane, dimethyl sulfoxide, DMF, DMP or other high-polarity aprotic solvents.

3. The process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile according to claim 1 , characterized in that the catalyst used for the catalytic addition of cyanuric fluoride and perfluoroolefin to generate trisperfluoroalkyl triazine is as follows: 5-20 wt % of NaF, KF, CsF, AgF or other fluorides, 0.1-2 wt % of tertiary amine, or 30-90 wt % of resins or other loading agents with tertiary amine, N-methylmorpholine or DABCO grafted on the surface.

4. The process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile according to claim 1 , characterized in that the trisperfluoroalkyl triazine is subjected to gasification and carried into a fixed bed reactor by a carrier gas for high-temperature catalytic cracking to obtain perfluoroalkyl nitrile, wherein the catalyst used in the fixed bed reactor is a metal salt loaded by a loading agent of alumina, molecular sieve, activated carbon, phosphomolybdic acid, or phosphotungstic acid.

5. The process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile according to claim 4 , characterized in that the metal salt is platinum, palladium or copper salt.

6. The process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile according to claim 4 , characterized in that the metal salt is copper nitrate, palladium chloride or chloroplatinic acid.

7. The process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile according to claim 4 , characterized in that the loading agent is phosphomolybdic acid or phosphotungstic acid.

8. The process for preparing environmentally-friendly insulating gas perfluoroalkyl nitrile according to claim 1 , characterized in that the molar ratio of cyanuric chloride to sodium fluoride in the fluorination reaction is 1:(3-10), and the reaction temperature is 80-160° C.; the molar ratio of cyanuric fluoride to perfluoroolefin in the catalytic addition is 1:(3-8), the reaction temperature is 80-220° C., the reaction time is 2-60 h, and the reaction pressure is 1.2-20 Bar; and the reaction temperature in the high-temperature catalytic cracking is 400-1000° C.

Assignees

• State Grid Corp China
• State Grid Shaanxi Electric Power Res Institute
• Univ Central South
• State Grid (Xi'An) Environmental Prot Technique Center Co Ltd

Inventors

• Sun Qiang
• Wu Jian
• Chen Yin
• Ding De
• Zhang Genzhou
• Bai Xiaochun
• Guo Anxiang
• Zhang Yantao
• Lv Pinghai
• Yu Xiaobing

Classifications

• C07C253/00 Primary

  Preparation of carboxylic acid nitriles (of cyanogen or compounds thereof C01C3/00) · CPC title

• C07D251/28

  Only halogen atoms, e.g. cyanuric chloride · CPC title

• C07D251/24

  to three ring carbon atoms · CPC title