Electrode and production method therefor, and production method for regenerated electrode

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.

1 . 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. 
     
     
         2 . The electrode according to  claim 1 , which 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 electrode according to  claim 1 , which is obtained by subjecting, to electrolytic nickel plating, a nickel component that has been 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 with use of an anode containing nickel as a base material, or the anode that has been worn in the nitrogen trifluoride production process. 
     
     
         4 . The electrode according to  claim 3 , which 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. 
     
     
         5 . The electrode according to  claim 1 , which is used to produce nitrogen trifluoride. 
     
     
         6 . A method for producing an electrode 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, or a nickel component that has settled in a molten salt, 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.   
     
     
         7 . The method for producing an electrode according to  claim 6 , 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.   
     
     
         8 . 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 . 
     
     
         9 . 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. 
     
     
         10 . A method for producing 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, or having settled in the molten salt, 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.   
     
     
         11 . 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 10 , and recovering a nickel component that has been deposited on a cathode during the production of nitrogen trifluoride, or a nickel component that has settled in a molten salt 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.   
     
     
         12 . 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. 
     
     
         13 . The electrode according to  claim 2 , which is obtained by subjecting, to electrolytic nickel plating, a nickel component that has been 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 with use of an anode containing nickel as a base material, or the anode that has been worn in the nitrogen trifluoride production process. 
     
     
         14 . The electrode according to  claim 2 , which is used to produce nitrogen trifluoride. 
     
     
         15 . The electrode according to  claim 3 , which is used to produce nitrogen trifluoride. 
     
     
         16 . The method for producing an electrode according to  claim 7 , 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 . 
     
     
         17 . 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. 
     
     
         18 . The method for producing an electrode according to  claim 8 , wherein, in the nickel plating, a fluorine ion concentration in the plating bath is 10 g/L or less. 
     
     
         19 . A regenerated electrode, which is regenerated using the production method according to  claim 11 , 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. 
     
     
         20 . The electrode according to  claim 13 , which is used to produce nitrogen trifluoride.