Method for producing fluorine gas

Patent metadata

Field	Value
Publication number	US-12358796-B2
Application number	US-202017595873-A
Country	US
Kind code	B2
Filing date	Aug 20, 2020
Priority date	Aug 30, 2019
Publication date	Jul 15, 2025
Grant date	Jul 15, 2025

Abstract

A method for producing fluorine gas including a fluorination step of obtaining a reaction mixture containing a major fluorinated substance that is a target component generated by fluorination of a raw material compound and by-product hydrogen fluoride, a separation step of separating the reaction mixture to obtain a main product component containing the major fluorinated substance and a by-product component containing the by-product hydrogen fluoride, a purification step of purifying the by-product component to obtain a recovered hydrogen fluoride component in which a concentration of an organic substance is reduced and a concentration of the by-product hydrogen fluoride is increased, an electrolysis step of performing electrolysis using the recovered hydrogen fluoride component as at least a part of an electrolyte to produce fluorine gas, and an introduction step of introducing the fluorine gas obtained in the electrolysis step into a reaction field for fluorination in the fluorination step.

First claim

The invention claimed is:

1. A method for producing fluorine gas comprising:
reacting 1,2,3,4-tetrachlorobutane or 1,1,2,2-tetrafluoroethane as a raw material compound with fluorine gas to perform fluorination and obtaining a reaction mixture containing 1,1,2,3,4,4-hexafluoro-1,2,3,4-tetrachlorobutane or perfluoroethane which is a major fluorinated substance as a target component generated by the fluorination of the 1,2,3,4-tetrachlorobutane or 1,1,2,2-tetrafluoroethane, a minor fluorinated substance as a non-target component generated as a by-product by the fluorination of the 1,2,3,4-tetrachlorobutane or 1,1,2,2-tetrafluoroethane, and by-product hydrogen fluoride generated as a by-product in the fluorination;
separating the reaction mixture to obtain a main product component containing the 1, 1,2,3,4,4-hexafluoro-1,2,3,4-tetrachlorobutane or perfluoroethane as a majority component and a by-product component, the by-product component being a component other than the main product component and containing the by-product hydrogen fluoride;
purifying the by-product component to obtain a recovered hydrogen fluoride component in which a concentration of an organic substance contained in the by-product component is reduced and a concentration of the by-product hydrogen fluoride is increased;
performing electrolysis using the recovered hydrogen fluoride component as at least a part of an electrolyte to produce fluorine gas; and
introducing the fluorine gas obtained in the electrolysis into a reaction field for the fluorination in performing the fluorination to use the fluorine gas obtained in the electrolysis as at least a part of fluorine gas used in the fluorination;
wherein, the by-product component is purified such that a total concentration of the organic substance in the recovered hydrogen fluoride component becomes 200 mass ppm or less.

2. The method for producing fluorine gas according to claim 1 , wherein the organic substance contained in the by-product component is at least one of the raw material compound that is not reacted, the minor fluorinated substance, a solvent caused to coexist with the raw material compound and the fluorine gas in the reaction field for the fluorination, a fluorinated substance of the solvent, a diluent gas caused to coexist with the raw material compound and the fluorine gas in the reaction field for the fluorination, a fluorinated substance of the diluent gas, an organic compound that is used in a reaction device in which the fluorination is performed and can be present in the reaction field, and a fluorinated substance of the organic compound.

3. The method for producing fluorine gas according to claim 1 , wherein the raw material compound is a compound having 2 or more and 18 or less carbon atoms and having 1 or more hydrogen atoms.

4. The method for producing fluorine gas according to claim 3 , wherein the compound having 2 or more and 18 or less carbon atoms and having 1 or more hydrogen atoms is an alkane or a halogenated alkane, and the halogenated alkane is an alkane in which a part or all of hydrogen atoms in the alkane are each substituted with a halogen atom other than fluorine.

5. The method for producing fluorine gas according to claim 1 , wherein a method for purifying the by-product component in the purification includes at least one of a distillation operation, an adsorption operation, and a liquid-liquid separation operation.

6. The method for producing fluorine gas according to claim 5 , wherein the distillation operation includes distilling a hydrogen fluoride aqueous solution obtained by causing the by-product hydrogen fluoride in the by-product component to be absorbed in water.

7. The method for producing fluorine gas according to claim 5 , wherein the adsorption operation includes causing the organic substance in the by-product component to be adsorbed to an adsorbent having at least one of activated carbon and alumina.

8. The method for producing fluorine gas according to claim 2 , wherein the raw material compound is a compound having 2 or more and 18 or less carbon atoms and having 1 or more hydrogen atoms.

9. The method for producing fluorine gas according to claim 2 , wherein a method for purifying the by-product component in the purification includes at least one of a distillation operation, an adsorption operation, and a liquid-liquid separation operation.

10. The method for producing fluorine gas according to claim 3 , wherein a method for purifying the by-product component in the purification includes at least one of a distillation operation, an adsorption operation, and a liquid-liquid separation operation.

11. The method for producing fluorine gas according to claim 4 , wherein a method for purifying the by-product component in the purification includes at least one of a distillation operation, an adsorption operation, and a liquid-liquid separation operation.

Assignees

• Showa Denko Kk
• Resonac Corp

Inventors

• Fujimura Koki
• Kobayashi Hiroshi
• FUKUCHI Yohsuke

Classifications

• C25B1/24

  Halogens or compounds thereof · CPC title

• C01B7/19

  Fluorine; Hydrogen fluoride · CPC title

• C01B7/20 Primary

  Fluorine · CPC title

• C25B15/081

  Supplying products to non-electrochemical reactors that are combined with the electrochemical cell, e.g. Sabatier reactor · CPC title

• C25B15/085

  Removing impurities · CPC title