Free powders as well as compacts of molybdenum and cobalt have been successfully recovered from spent hydrogenation and desulphurisation catalysts. A mixture of concentrated sulphuric and nitric acids (3: 1 by volume) achieved adequate levels of recovery of both metals, which increased with increase in acid concentration, time (up to 3 h), and temperature (100°C), and with decrease in particle diameter of the spent catalyst. The process flow sheet involved crushing, milling, particle sizing, acid leaching, and roasting of the obtained hydroxides in an atmospheric oxygen to obtain the respective oxides. These were reduced under a constant mass flowrate of hydrogen gas at 1100 and 900°C respectively. Parameters affecting the properties of the products and the recovery efficiency value, such as acid concentration, particle diameter of the solid catalyst, temperature, and time, have been investigated. The results obtained showed that the maximum recovery efficiency amounted to 96%. The recovered metal powders are technically pure, meeting the standard specifications. Compact shapes of molybdenum acquired density values which increased with an increase of the pressing load, whereby a density value of 2280 kg m−3 is attained at ≥0 ·75 MPa. A model explaining the obtained results assumes that the molybdenum and cobalt in the spent catalyst are supported by the carrier. During operation, carbon particles are deposited and poison the catalyst. The weight ratio of carbon increases as the particle size of the catalyst decreases. Nitric acid helps dissolution of these metals to form complex sulphate salts. High oxide states of molybdenum and cobalt are formed by roasting in atmospheric oxygen. Reduction with hydrogen gas takes place in two steps, the overall activation energy of which amounts to 144·39 kJ mol−1 for molybdenum and 143·4 kJ mol−1 for cobalt. The metal powders have a rough surface with an irregular shape. Densification of these powders by pressing takes place as a result of random movement of the metal particles. Above a critical load, the minimum void volume is achieved at which the interparticle friction resists the applied load. A study has revealed that spent catalyst contains molybdenum and cobalt that are economically recoverable. Cost of recovery and the process of recovery is simple. PM/0709