Zhenxing Ren, Lizhen Lian, Xingle Zuo, Xin Cui, Min Zhang, Liu Deng, Liqiang Wang, You‐Nian Liu
Abstract Copper‐based catalysts are attractive for hydrogenation, exemplified by nitro‑group reduction to industrially important aromatic amines, but are limited by intrinsically weak H 2 activation arising from an inert electronic structure. Herein, a dual‐site catalyst is developed by integrating FeN 4 and defect‐rich Cu 1.81 S nanoparticles anchored on porous carbon (Cu 1.81 S/Fe 1 @PC) via a protein‐metal ion network‐derived route. Cu 1.81 S/Fe 1 @PC features a high specific surface area (1130 m 2 g −1 ) and a unique N, S‐codopant structure. Density functional theory reveals electron transfer from FeN 4 to Cu 1.81 S, and the abundant lattice defects in Cu 1.81 S, which lower the H─H dissociation barrier on Cu sites. At 120 °C and 10 bar H 2 , the as‐prepared Cu 1.81 S/Fe 1 @PC catalyst delivers >99% aniline yield with a turnover frequency of 625 h −1 , ranking among the most active Cu‐ or Fe‐based catalysts for nitroarene hydrogenation. This work provides a new approach for designing and preparing high‐performance dual‐site catalysts, applicable to, but not limited to, hydrogenation reactions.