Reactions of Mo compounds and their combinations with the salts of Ni or Co, in the fluxes containing sulfur and alkali metal carbonates in the temperature range 300-400degreesC, lead to the formation of dispersed simple or mixed Mo sulfides. For the reaction of ammonium heptamolybdate (AHM) and sodium carbonate, depending on the conditions, pure MoS2 or intercalated phase Na0.3MoS3 was obtained. Cobalt-containing mixed sulfide with the structure Of MoS2 was prepared, having a specific surface area of 75 m(2) g(-1) and demonstrating a high activity in the thiophene hydrodesulfurization (HDS) model catalytic test. (C) 2002 Elsevier Science B.V. All rights reserved.