Production of High‐Purity 2,5‐Furandicarboxylic Acid through Electrocatalytic Oxidation of 2,5‐Bis(hydroxymethyl)furan over Reconstructed Ni2P/NF

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, a unique Ni 2 P/NF catalyst is designed using a chemical vapor deposition method along with a rapid reconstruction (Ni 2+ → Ni 3+ ) rate, stably achieving ≈90% FDCA yields from BHMF electron‐oxidation after 10 cycles at a formation rate of 218 μmol FDCA cm −2 h −1 (seven times higher than data in reported literature). The abundance of available electrons near the Ni‐3 d Fermi level, together with the reduced NiP bond strength and the lowest electronegativity of Ni 2 P, accelerates 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.