Hydrometallurgical recovery of nano-palladium (Pd) from spent Pd/Al 2 O 3 catalyst has been investigated. The Pd content in the spent catalyst sample was assayed to be 0.42% while the remainder was mainly aluminum oxide. Mixture of HCl and AlCl 3 was studied as leaching agent for the sample. The Pd was deposited with formic acid. Different parameters affecting leaching and deposition processes such as, time, temperature, liquid/solid ratio, were investigated. Phase of spent catalyst were identified by X-ray diffraction (XRD) analysis. The deposited Pd was characterized by scanning electron microscope (SEM), transmission electron microscope (TEM) and energy dispersive X-ray (EDX) for identification of the grain size and composition. The deposited palladium was found to be in the nano-size range (34.5-70.5 nm).