A simple method for preparing highly active and dispersed supported metal catalysts was developed by co-impregnation. Compared with conventional wetness impregnation, addition of moderate ethylene glycol into the metal nitrate aqueous solution could enhance interaction with MCM-41 surface, resulting in formation of very small NiO particle size (3.5 nm) and high dispersion of the active phase. The Ni/MCM-41 catalysts using co-impregnation exhibited excellent catalytic performance for low temperature hydrogenation of naphthalene with 100% conversion at 55 °C, which could rival the activity of commercial Raney Ni catalyst. The obtained catalysts were characterized by XRD, TEM, TG-DSC, FT-IR, BET and TPR.