One-Step Hydrothermal Synthesis of Ni2P/MIL-53(Fe) and Its Catalytic Performance in the Selective Oxidation of Aromatic Alcohols

Developing cost-effective photocatalysts with high activity remains a key challenge in photocatalysis. In this study, a low-cost nickel phosphide (Ni2P) cocatalyst was combined with MIL-53(Fe) to fabricate Ni2P/MIL-53(Fe) nanocomposites via a simple hydrothermal method. The as-prepared composites were systematically characterized by XRD, FT-IR, SEM, UV-vis DRS, PL, and EIS to evaluate their structural, morphological, optical, and electrochemical properties. The introduction of Ni2P significantly promoted the separation of photogenerated electron–hole pairs on the MIL-53(Fe) surface, thereby enabling valence band holes (h+) to participate in alcohol oxidation, as confirmed by photoelectrochemical analysis. Under optimized conditions, the Ni2P/MIL-53(Fe) nanocomposite achieved a significant photocatalytic alcohol conversion rate of 74%, which is 7.4-fold and 2.5-fold higher than those of pristine Ni2P and MIL-53(Fe), respectively. Furthermore, mechanistic studies revealed that valence band holes are primarily responsible for the selective oxidation of aromatic alcohols.