With the aim of disposing hazardous sulphur-containing chemicals, an experimental investigation on the hydrodesulfurization (HDS) of the model compound dibenzothiophene (DBT) is presented. Mesoporous NiMo-Al2O3 catalysts for HDS were prepared by efficient and simple one-pot synthesis method using aluminum chloride as start material, urea as precipitant and starch as template. The catalysts were characterized by means of N-2 physisorption, XRD, SEM, TPR, XPS and HRTEM. The characterization results show that, compared with the NiMo/Al2O3 catalysts prepared by impregnation method, the as-prepared NiMo-Al2O3 catalysts exhibit smaller nano-sized spherical particles of alumina, higher dispersions of Ni and Mo species, shorter length and lower stacking layer number of MoS2 slabs. Thus, NiMo-Al2O3 catalysts possess higher catalytic performance in the HDS of DBT than those of impregnated catalysts. Therefore, one pot synthesis is a promising method for the development of hydrotreating catalysts. (C) 2013 Elsevier B.V. All rights reserved.