Fabrication of a Novel Nanoporous FeSiB Powder Catalyst via Annealing–Dealloying Synergistic Strategy for Enhanced p-Nitrophenol Degradation

p-Nitrophenol (PNP), a highly toxic and recalcitrant organic pollutant prevalent in industrial wastewater, poses severe challenges to traditional Fenton treatment technologies. In this study, a novel nanoporous catalyst is synthesized via a combined annealing–dealloying strategy. Annealing at 550 °C and 600 °C induces partial crystallization, generating α-Fe and Fe2B phases that serve as preferential corrosion sites during chemical dealloying. This process results in a three-dimensionally interconnected nanoporous structure, which significantly increases the specific surface area of the catalyst to 2.642 m2/g. The optimized nanoporous catalyst exhibits excellent degradation performance, achieving complete removal of PNP within 30 min under room temperature reaction conditions. Notably, kinetic analysis reveals a degradation mechanism involving adsorption and Fenton-like catalysis. The high specific surface area provides abundant active sites for PNP adsorption, while the enhanced Fe2+ dissolution synergistically accelerates the degradation. The adsorption kinetic follows a pseudo-second-order model, and the degradation kinetic conforms to a first-order model, with activation energy analysis further confirming a surface-reaction-controlled process. This work provides a feasible approach and technical reference for designing efficient porous catalysts based on amorphous alloys for advanced treatment of refractory organic wastewater.