Catalysts based upon ZSM-5 zeolites (SiO2/Al2O3 molar ratio of 30 and 150) were synthesized and tested for the carbon disulfide (CS2) conversion. First, the zeolites were shaped in pellets using alumina (20wt%) as binder. The pellets containing ZSM5 (SiO2/Al2O3=30) were exchanged with Co2+. Afterwards, this material and the other one, having the zeolite with SiO2/Al2O3 ratio of 150, were co-impregnated with Mo and Co salts. The structural variations were explored by means of X-Ray Diffraction. The progressive reduction of the metal phases was studied by Thermal Programmed Reduction (TPR): the acidity distribution was evaluated by FTIR-pyridine adsorption and the aggregation state of the crystalline phases was characterized by High Resolution Transmission Electron Microscopy (HRTEM) and EDS. The catalytic properties were evaluated in a fixed bed reactor at 350 degrees C, P = 20 kg/cm(2) with a H-2/CS2 molar ratio equal to 2. The results suggest a hindering of catalytic activity by the metal phase, which is deposited either on the alumina or over the external surface of the zeolite crystallites. (C) 2009 Elsevier B.V. All rights reserved.