Electrosynthesis of Co‐doped Cu mesh Catalyst for HMF Oxidation Reaction

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. Herein, an electrochemical synthesis strategy was employed to synthesize bimetallic Co‐doped Cu mesh catalyst for HMF oxidation reaction. It exhibited a remarkable electrooxidation activity during 3‐hour reaction at 1.6 V vs. 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 Co3O4 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 towards FDCA.