Electrode production method

Patent metadata

Field	Value
Publication number	US-2022411949-A1
Application number	US-202217823548-A
Country	US
Kind code	A1
Filing date	Aug 31, 2022
Priority date	Sep 6, 2017
Publication date	Dec 29, 2022
Grant date	—

Abstract

An electrode for electrolytic fluorination contains nickel as a base material with a fluorine content<1,000 ppm. Preferably, in at least a surface portion thereof, the nickel content>99 mass %, the iron content≤400 ppm, the copper content<250 ppm, and the manganese content<1,000 ppm. A method for producing an electrode includes arranging a nickel base material electrode in a nickel plating bath as a cathode, and applying nickel plating to the nickel base material electrode by electrolytic nickel plating, the method including (1) using, as an anode, a nickel component deposited on a cathode, or a nickel component that has settled in a molten salt, in a process of producing nitrogen trifluoride by molten salt electrolysis using a nickel base material anode, or the nickel base material anode; or (2) using, as the cathode, the nickel base material anode.

First claim

1 . A method for producing an electrode for fluorinating a compound by electrolysis, the electrode containing nickel as a base material and having a fluorine content of less than 1,000 ppm, and
the method comprising subjecting, to electrolytic nickel plating, a nickel component that has been deposited on a cathode in a process of producing nitrogen trifluoride by molten salt electrolysis with use of an anode containing nickel as a base material, or the anode that has been worn in the nitrogen trifluoride production process to obtain the electrode.

2 . The method for producing an electrode according to claim 1 , wherein the electrode has, in at least a surface portion thereof, a nickel content of 99 mass % or more, an iron content of 400 ppm or less, a copper content of 250 ppm or less, and a manganese content of 1,000 ppm or less.

3 . The method for producing an electrode according to claim 1 , wherein the electrode is obtained by electrodepositing the nickel component that has been deposited on the cathode in the nitrogen trifluoride production process, onto a nickel base material by electrolytic nickel plating.

4 . The method for producing an electrode according to claim 1 , wherein the electrode is used to produce nitrogen trifluoride.

5 . The method for producing an electrode according to claim 1 by disposing a nickel base material in a nickel plating bath as a cathode and applying nickel plating to the nickel base material by electrolytic nickel plating, the method comprising (1) or (2) below:
(1) using, as a nickel component that is arranged in the nickel plating bath as an anode, a nickel component that has been deposited on a cathode in a process of producing nitrogen trifluoride by molten salt electrolysis with use of an anode containing nickel as a base material, or a nickel base material electrode that has been used as the anode in the nitrogen trifluoride production process; and
(2) using, as the nickel base material that is arranged in the nickel plating bath as the cathode, the nickel base material electrode that has been used as the anode in the process of producing nitrogen trifluoride by molten salt electrolysis.

6 . The method for producing an electrode according to claim 5 , wherein a nickel base material electrode is used as the cathode in the process of producing nitrogen trifluoride, and
a nickel component that has been deposited on the cathode is used in the nickel plating.

7 . The method for producing an electrode according to claim 5 , wherein, in the nickel plating, a pH of the plating bath is set to be from 1.0 to 5.0, and a current density is set to be from 1.0 to 6.0 A/dm 2 .

8 . The method for producing an electrode according to claim 5 , wherein, in the nickel plating, a fluorine ion concentration in the plating bath is 10 g/L or less.

9 . A method for producing the electrode according to claim 1 which is a regenerated electrode by regenerating a nickel base material electrode which has been used as an anode in order to fluorinate a compound by electrolysis and in which nickel has been worn, the method comprising the steps of:
recovering a nickel component out of a molten salt, the nickel component having been deposited on a cathode in a process of producing nitrogen trifluoride by molten salt electrolysis with use of an anode containing nickel as a base material; and
electrodepositing the recovered nickel component onto a surface of the worn nickel base material electrode to thereby regenerate the nickel base material electrode.

10 . A method for producing a regenerated electrode, the method comprising the steps of:
using, as an anode in producing nitrogen trifluoride by molten salt electrolysis, an electrode that is regenerated using the production method according to claim 9 , and recovering a nickel component that has been deposited on a cathode during the production of nitrogen trifluoride out of the molten salt; and electrodepositing the recovered nickel component onto a surface of the electrode that has been worn after the regeneration, to thereby regenerate the electrode.

11 . The method for producing the electrode according to claim 9 , wherein the regenerated electrode is regenerated using the production method according to claim 9 , wherein a mass of the regenerated electrode after the regeneration is larger than a mass of the worn nickel base material electrode prior to the regeneration by 10 mass % or more.

12 . The method for producing an electrode according to claim 2 , wherein the electrode is used to produce nitrogen trifluoride.

13 . The method for producing an electrode according to claim 6 , wherein, in the nickel plating, a pH of the plating bath is set to be from 1.0 to 5.0, and a current density is set to be from 1.0 to 6.0 A/dm 2 .

14 . The method for producing an electrode according to claim 6 , wherein, in the nickel plating, a fluorine ion concentration in the plating bath is 10 g/L or less.

15 . The method for producing an electrode according to claim 7 , wherein, in the nickel plating, a fluorine ion concentration in the plating bath is 10 g/L or less.

16 . A method for producing an electrode, the electrode being a regenerated electrode which is regenerated using the production method according to claim 10 , wherein a mass of the regenerated electrode after the regeneration is larger than a mass of the worn nickel base material electrode prior to the regeneration by 10 mass % or more.

Assignees

• Kanto Denka Kogyo Kk

Inventors

• Okubo Kimitaka

Classifications

• C01B21/083

  containing one or more halogen atoms · CPC title

• C01B21/0835

  Nitrogen trifluoride · CPC title

• C25B1/245 Primary

  Fluorine; Compounds thereof · CPC title

• C25B11/042

  Electrodes formed of a single material · CPC title

• C25B9/09

  Fused bath cells · CPC title