Metal recovery from spent catalysts minimizes the volume of hazardous waste disposed of in landfills and is an alternative to conventional mining. The objectives of this dissertation are to characterize a spent catalyst residue used in the methanol synthesis process and to determine a route for copper and zinc recovery from this residue. The components that correspond to the active phase, promotor, and support of the spent catalyst were identified as copper, zinc, and aluminum, respectively. Which presented themselves as CuO, Zn3O(SO4)2, and Al2O3. The physical technique of separation through dense media, with the use of bromoform, and the pyrometallurgical techniques of reduction, zinc volatilization, and copper fusion were studied. Before the best techniques investigation, the spent catalyst was pre-treated by calcining and grinding. The parameters studied in the reduction and volatilization step were temperature, holding time, type of reducer, gas flow, and furnace rotation. In the melting step, the parameters studied were the proportion of the oxides Al2O3, CaO, and SiO2 and the amount of the fondant CaF2. The best zinc extraction obtained from the reduction and volatilization tests was 92.9% in a test carried out at 1100°C for 6 hours, with the graphite reducer, without rotation, and inert atmosphere with argon at 100mL/min. The purity of the condensed and recovered zinc in the cold finger was 80.9%. The best copper recovery test was the melt, which separated 72.4% of the metal from the rest of the sample with a purity of 73.3%. The result was achieved with the lowest proportion of silica and the highest proportion of CaF2. The sequence of techniques that presented the best metal recovery results was pre-treatment by calcining and grinding, followed by a step of reduction, zinc volatilization, and copper melting.