Various ratio of Co-Ag supported on ZnO have been evaluated in the selective catalytic oxidation of styrene to benzaldehyde, using H 2 O 2 as an oxidant. e catalysts were prepared by a sol-gel process and were characterized using XRD, FT-IR, TG-DTG, BET, and SEM/EDX. e performance of the prepared catalyst was investigated under different parameters such as solvent, temperature, substrate/oxidant molar ratios, reaction time, and doping percent. e Zn 1−x−y Ag x Co y O catalysts exhibit a good activity and a high selectivity towards benzaldehyde (95%) with the formation of only 5% of acetophenone.