Bismuth-based modified electrode, manufacturing method thereof and use thereof

Patent metadata

Field	Value
Publication number	US-12435432-B2
Application number	US-202217934541-A
Country	US
Kind code	B2
Filing date	Sep 22, 2022
Priority date	Jul 4, 2022
Publication date	Oct 7, 2025
Grant date	Oct 7, 2025

Abstract

A modified electrode, manufacturing method thereof and use thereof are provided. The manufacturing method includes steps of soaking a copper substrate in a solution to obtain a BiOI/copper(I) iodide, BiOI/copper(I) iodide/metallic bismuth, and copper(I) iodide/metallic bismuth composite modified electrodes by electroless plating method. The obtained electrodes, designated as bismuth-based modified electrode, can be used for the electrohydrodimerization of acrylonitrile to synthesize adiponitrile.

First claim

What is claimed is:

1. A method of manufacturing a bismuth-based modified electrode, comprising a step of:
immersing a copper substrate in an aqueous solution for 1 to 20 minutes to obtain the bismuth-based modified electrode;
wherein the aqueous solution comprises a bismuth solution and KI solution, and a concentration of the KI solution ranges from 0.4 M to 3.0 M, and the bismuth solution comprises bismuth nitrate, bismuth carbonate, bismuth acetate, or bismuth citrate, and a concentration of the bismuth nitrate, a concentration of the bismuth carbonate, a concentration of the bismuth acetate, and a concentration of the bismuth citrate range from 20 mM to 40 mM, respectively,
wherein the aqueous solution further comprises an oxidizing agent and the oxidizing agent comprises p-benzoquinone with a concentration between 0.5 mM and 50 mM, hydrogen peroxide with a concentration between 1 mM and 10 mM, or 2,2′-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) diammonium salt with a concentration between 1 mM and 10 mM; and
immersing the copper substrate in an electrolyte with a concentration of 0.1 M and a pH between 7.0 and 9.2, and performing an electrochemical reduction at an applied potential between −0.5 V and −1.75 V vs. NHE for 30 minutes to 2 hours,
wherein the electrolyte is selected from the group consisting of phosphate solution, borate solution, and carbonate solution.

2. The method according to claim 1 , wherein the concentration of the KI solution is 0.4 M, and the bismuth solution comprises 40 mM bismuth nitrate, 20 mM bismuth carbonate, 40 mM bismuth acetate, or 40 mM bismuth citrate.

3. The method according to claim 1 , wherein the oxidizing agent comprises 50 mM p-benzoquinone, 5 mM hydrogen peroxide, or 5 mM 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt.

4. The method according to claim 1 , wherein the copper substrate is immersed in 0.1 M borate buffer, pH 9.2.

5. The method according to claim 1 , wherein the electrochemical reduction is performed at the applied potential at −1.745 V vs. NHE for 30 minutes.

6. The method according to claim 1 , wherein the copper substrate is immersed in the aqueous solution for 4 minutes.

Assignees

• Univ Nat Cheng Kung

Inventors

• Lin Chia-Yu
• Su Chia-Sheng
• Yen Chia-Hui
• Huang Shih-Ching
• Lu Wei-Hsin

Classifications

• C23C18/1646 Primary

  Characteristics of the product obtained · CPC title

• C25B11/052

  Electrodes comprising one or more electrocatalytic coatings on a substrate · CPC title

• C25B3/09

  Nitrogen containing compounds · CPC title

• C25B3/295

  hydrodimerisation · CPC title

• C25B11/061

  Metal or alloy · CPC title