This paper presents the results of a study on the catalytic activity and selectivity of nickel and palladium catalysts in hydrogenation reactions of nitro- and acetylene compounds. It was shown that the activity and selectivity of nickel catalysts in the hydrogenation of phenylacetylene depend on the nature of modifying additives (Cu, Zn, Ti, Cr, Bi, Ti–Cu, Mn, Fe), and the activity and selectivity of palladium catalysts based on a polymer of metal complexes depends on the method of their preparation. It was found that for certain concentrations of the active phase of palladium (0.8 wt.%) and the polymer of potassium humate (1.0 wt.%.) in the catalyst, where palladium and the polymer were deposited on bauxite-094 together, the catalyst exhibits the greatest activity and selectivity when hydrogenating phenylacetylene and potassium orthonitrophenolate.