A Study on the recovery of the valuable metals(Vanadium Molybdenium) was carried out using spent catalysts originated from desulfurizing process of oil refinery. Experiments consisted of pre-roasting for Sulfur and Carbon removal, soda roasting and leaching for the extraction of valuable metals, and selective precipitation of Vanadium and Molybdenium. Effects of temperature and time in roasting for Sulfur removal, of $Na_2CO_3$ concentrations in soda roasting, and of pulp density, temperature and time in leaching were investigated for the recovery of Vanadium and Molybdenium. A optimum condition having over 85% in yield of Vanadium and Molybdenium was found. In the selective precipitation, more than 98% of Vanadium and Molybdenium were obtained by the variation of pH and concentration of additives.