Electrochemical biomass oxidation holds great promise for replacing oxygen evolution reaction (OER) in water splitting process due to its lower thermodynamic energy barrier. Among the various biomass-derived intermediates, 5-hydroxymethylfurfural (HMF) stands out as the pivotal chemical platform with immense potential, as it can be subjected to produce value-added chemicals and diminish the reliance of fossil fuels. However, there has been limited research on the electrochemical HMF oxidation reaction (HMFOR) specifically focused on the production of intermediate products. In this study, the efforts were directed towards developing the non-precious metal-based catalyst to selectively produce value-added intermediate products using V-doped Ni(OH)2 in mildly alkaline medium (pH 9.4). Among all, the optimized V0.15 -Ni(OH)2 has been developed and exhibited high catalytic activity with ~60% selectivity towards the production of 5formyl furan-2-carboxylic acid (FFCA) or 2,5-diformylfuran (DFF), depending on the reaction parameters, with nearly 100% Faradaic efficiency. The incorporation of V into the Ni(OH)2 lattice is shown to trigger the phase transition of -Ni(OH)2 to -Ni(OH)2 and endow the catalyst with rougher structure which promotes more active sites. Benefiting from this, the optimized V0.15-Ni(OH)2 has 1.7 times higher yield as compared to its counterparts tested under the same reaction parameters. Combining the in-situ Raman and ex-situ X-ray photoelectron spectroscopy results, the V incorporation facilitated the higher formation of Ni3+ and introduced structural disorder which are the fundamental features that account for the enhanced performance. Furthermore, this study also extended to the effect of different anion electrolyte (B4O72-, CO32-, and PO43-) towards electrochemical HMFOR which found to have the ability to affect the stability of the catalyst, reaction kinetics, charge transfer rate and probably interfacial pH. Thus, this study not only opens avenues for selective HMF oxidation to value-added intermediate products by improving catalyst design but also evaluates the impact of reaction parameters.

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