High‐purity FDCA production over reconstructed Ni2P/NF via electrocatalytic oxidation of BHMF

The generation of high‐valence surface active species (such as CoOOH and NiOOH) determines the crucial oxidation rates and stabilities in the electrocatalytic reactions. Herein, we designed a unique Ni2P/NF catalyst with a chemical vapor deposition method along with a rapid reconstruction (Ni2+→Ni3+) rate, stably achieving ca. 90% FDCA yields from BHMF electron‐oxidation after 10 cycles at a formation rate of 218 μmolFDCAcm‐2h‐1 (seven‐times higher than data in reported literature). The abundance of available electrons near the Ni‐3d Fermi level, together with the reduced Ni‐P bond strength and the lowest electronegativity of Ni2P, accelerate surface NiOOH species formation. In addition, the electrocatalytic oxidation of BHMF offers a more stable furan‐based substrate, while also prolonging the residence time of the oxidative intermediate HMF. This mitigates humin formation, thereby enabling the synthesis of high‐purity FDCA (>99%) at high concentrations (100 mmol L‐1), making it a promising approach for efficient FDCA synthesis.