In this study, we report the synthesis of a highly reactive and recyclable catalyst for the aqueous-phase reduction of 4-nitrophenol (4-NP) using dual-cation incorporated Pd nanocubes. Fe and Ce cation-doped Pd nanocubes (PdFeCe) were synthesized via cation exchange under mild conditions. Dual-cation incorporation effectively regulates the lattice structure and electronic interactions, providing more active sites than single metal-doped or pure Pd nanocubes. Aminoclay (AC), with excellent aqueous dispersibility, was used as a support, enhancing the recyclability of the catalyst. The PdFe 15 Ce 5 /AC catalyst exhibited superior reactivity compared to carbon-supported and commercial catalysts, demonstrating significant reactivity, stability, and recyclability improvements.