Two different strategies have been designed for the acid and alkaline leaching steps of hydrodesulphurization catalysts. Tests have been performed on out-of-range catalysts issued from catalyst manufacturing process. Experimental conditions have been screened for these different processes considering the effects of concentration, temperature, solid/ liquid ratio, etc. The best conditions have been used for producing two leachates that were treated by precipitation for recovery of valuable metals such as cobalt and molybdenum. Post-treatments have also been designed for the selective separation of Co from Mo: X-ray diffraction analyses on selective precipitates (as sulfide) confirm the purity of produced materials. Two flow sheets are proposed that allow selectively recovering more than 95% of the valuable metals.