Electrosynthesis of Co‐Doped Cu Mesh Catalyst for HMF Oxidation Reaction

Abstract The growing demand for sustainable alternatives to fossil‐derived chemicals has spurred significant interest in biomass valorization, with 5‐hydroxymethylfurfural (HMF) emerging as a key platform molecule. In this study, an electrochemical synthesis strategy was employed to synthesize a bimetallic Co‐doped Cu mesh catalyst for the HMF oxidation reaction. It exhibited remarkable electrooxidation activity during a 3‐h reaction at 1.6 V versus RHE with 83.2% HMF conversion, 99.4% 2,5‐furandicarboxylic acid (FDCA) selectivity, and 87.7% Faraday efficiency. X‐ray diffraction, in situ surface‐enhanced Raman spectroscopy, and X‐ray photoelectron spectroscopy revealed that the modified Cu mesh catalyst introduced more Co 3 O 4 species. Additionally, in situ attenuated total reflection surface‐enhanced infrared absorption spectroscopy elucidated that Cu species on the Co‐doped Cu mesh can adsorb *OH and couple with organic molecules during the reaction process. Cu─Co dual active sites enhance the selective electrochemical oxidation of HMF toward FDCA.