IP Library Granted Patent US 12,358,796
Granted Patent B2
US 12,358,796 · App. 17/595,873 · Granted Jul 15, 2025

Method for producing fluorine gas

Inventors: Koki Fujimura (Tokyo, JP); Hiroshi Kobayashi (Tokyo, JP); Yohsuke Fukuchi (Tokyo, JP)
Assignee: Resonac Corporation
C01B7/20C01B7/19C25B1/24
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Quick Facts
Patent No.
US 12,358,796
App. No.
17/595,873
Granted
Jul 15, 2025
Kind
B2
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.

Claims (17)

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.

Assignments (3)
CHANGE OF ADDRESS Recorded Feb 9, 2024
From: RESONAC CORPORATION
To: RESONAC CORPORATION
Reel/Frame 066547/0677 →
CHANGE OF NAME Recorded Jun 23, 2023
From: SHOWA DENKO K.K.
To: RESONAC CORPORATION
Reel/Frame 064082/0513 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 29, 2021
From: FUJIMURA, KOKI; KOBAYASHI, HIROSHI; FUKUCHI, YOHSUKE
To: SHOWA DENKO K.K.
Reel/Frame 058228/0372 →