# US 2026/0098352 A1 · Metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode and method of preparing the same and method of preparing adiponitrile using metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2026/0098352 A1 - Document ID: US20260098352A1 - Status: Published application - Kind: A1 - Application number: 18/974,851 - Filed: 2024-12-10 - Published: 2026-04-09 - Earliest claimed: 2024-10-09 - Assignees: National Cheng Kung University - Applicants: National Cheng Kung University - Inventors: Chia-yu LIN; Shih-ching HUANG; Ming-chi TSAI; Wei-che TSAI - Web page: https://patentgrep.com/patent/US20260098352A1 ## CPC - C25B 11/091: consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds - C25B 3/09: Nitrogen containing compounds - C25B 11/069: consisting of at least one single element and at least one compound; consisting of two or more compounds - C25B 15/031: pH - C25B: ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR (anodic or cathodic protection C23F13/00; single-crystal growth C30B) ## Abstract A method of preparing a metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode is disclosed. The method comprises steps of: preparing a plating solution containing 0.25 M ammonium chloride, 0.067 M to 0.133 M nickel chloride, 0.067 M to 0.133 M ferrous sulfate, and 0.04 M to 2 M sodium hypophosphite; placing a copper iodide-bismuth composite electrode in the plating solution for electrodepositing metallic nickel/nickel-iron hydroxide catalytic layer onto the copper iodide-bismuth composite electrode to obtain the metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode, CuI—Bi/Ni—NiFe(OH)x(r), wherein r is a molar ratio of nickel chloride to ferrous sulfate. A metallic nickel/nickel-iron hydroxide catalytic layer modified copper iodide-bismuth composite electrode and a method of preparing adiponitrile using the metallic nickel/nickel-iron hydroxide catalytic layer modified copper iodide-bismuth composite electrode are further disclosed. ## Claims ### Claim 1 A method of preparing a metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode, comprising steps of: preparing a plating solution containing 0.25 M ammonium chloride, 0.067 M to 0.133 M nickel chloride, 0.067 M to 0.133 M ferrous sulfate, and 0.04 M to 2 M sodium hypophosphite; placing a copper iodide-bismuth composite electrode in the electroplating solution to deposit metallic nickel/nickel-iron hydroxide catalytic layer onto the copper iodide-bismuth composite electrode, resulting in a metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode, CuI—Bi/Ni—NiFe(OH)x(r), wherein r is a molar ratio of nickel chloride to ferrous sulfate. ### Claim 2 (depends on 1) The method as claimed in claim 1, wherein the metallic nickel/nickel-iron hydroxide catalytic layer is electroplated onto the copper iodide-bismuth composite electrode at a constant current density of −10 mA cm−2. ### Claim 3 (depends on 1) The method as claimed in claim 1, wherein a time of depositing the metallic nickel/nickel-iron hydroxide catalytic layer onto the copper iodide-bismuth composite electrode ranges from 10 seconds to 60 seconds. ### Claim 4 (depends on 1) A metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode, CuI—Bi/Ni—NiFe(OH)x(r), prepared by the method as claimed in claim 1, wherein r is a molar ratio of nickel chloride to ferrous sulfate. ### Claim 5 (depends on 4) A method of preparing adiponitrile using the metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode as claimed in claim 4, comprising a step of: electrolyzing acrylonitrile at a constant current density of −100 mA cm−2 to −400 mA cm−2 in a phosphate buffer containing 0.6 M to 0.8 M acrylonitrile, using the metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode as claimed in claim 4, to synthesize adiponitrile. ### Claim 6 (depends on 5) The method as claimed in claim 5, wherein the metallic nickel/nickel-iron hydroxide catalytic layer-modified copper iodide-bismuth composite electrode is modified by electrodepositing a metallic nickel/nickel iron hydroxide catalytic layer with a charge passage ranging from 0.1 C cm−2 to 0.6 C cm−2. ### Claim 7 (depends on 5) The method as claimed in claim 5, wherein a concentration of the phosphate buffer is 0.5 M and a pH of the phosphate buffer is 8. ### Claim 8 (depends on 5) The method as claimed in claim 5, wherein the phosphate buffer further contains 20 mM to 40 mM quaternary ammonium salt, and the quaternary ammonium salt is represented by formula (I): wherein R1 to R4 are each independently a C2-5 hydrocarbon group, and X− is ClO4−, H2PO4−, or Br−. ### Claim 9 (depends on 5) The method as claimed in claim 5, wherein electrolysis of acrylonitrile is carried out in a H-type electrochemical cell or a flow-type electrolyzer. ### Claim 10 (depends on 9) The method as claimed in claim 9, wherein a flow rate in the flow electrolysis system is 722 sccm.