In Situ Reconstruction of NiCo–MOF Enhances Acetate Production Through Ethanol Electro‐Oxidation in Alkaline Medium

Electrochemical ethanol oxidation (EOR) is promising strategy for value‐added chemical production, such as acetic acid, while replacing energy intensive oxygen evolution reaction at the anode. However, developing efficient, affordable electrocatalysts is crucial for practical ethanol electrolysis to enhance the EOR kinetics, reduce overpotential, and minimize energy losses. In this context, we synthesized a nickel‐cobalt‐based metal‐organic framework (NiCo–MOF) as a precatalyst for ethanol oxidation. The NiCo oxyhydroxides were formed by the in situ reconstruction of the MOF during the cycling process. This reconstructed composite exhibits outstanding electrocatalytic performance toward EOR, achieving a current density of 10 mA/cm 2 at 1.33 V (RHE). The reconstructed NiCo–MOF showed a maximum FE of ∼95.6% for acetate production at 50 mA/cm 2 current density. The better catalytic activity of reconstructed NiCo–MOF compared to other samples is due to its strong synergistic interaction between Ni and Co, which facilitates the preoxidation, thereby increasing the EOR. The catalyst also possesses a stable ethanol electrolysis through 50 h. The overall ethanol electrolysis on the catalyst needs 220 mv less potential compared to water electrolysis at 10 mA/cm 2 current density. The result suggests that in situ reconstructed bimetallic MOF could be an efficient electrocatalyst for alcohol electrooxidation for potential green energy integration.