Defined hexagonal cylindrical pore structure SBA-15 material was synthesized as support for hydrotreating catalysts. The stability of the mesoporous material under acid and basic environments commonly used to prepare hydrotreating catalysts was investigated. The effects of the acid and basic treatments on the stability of SBA-15 and NiMo/SBA-15 catalysts were evidenced by different characterization techniques such as N-2 adsorption-desorption, X-ray diffraction (XRD), Raman Spectroscopy and high resolution transmission electron microscopy (HRTEM). Supported NiMo/SBA-15 catalysts prepared by pore volume co-impregnation in acidic, neutral and basic solutions of the Ni and Mo precursor salts were characterized to evaluate the textural and structural changes caused by the method of preparation. Characterization of the support after accelerated stability tests indicates large deterioration of the SBA-15 structural order at basic pH. The characterization results of oxide and sulfided catalysts indicate, for the catalysts prepared at high pH, an increasing presence of beta-NiMoO4 phase in the oxide catalysts, and a relatively lower population of MoS2 in the sulfided catalysts. The activity of the different catalysts evaluated in the thiophene hydrodesulfurization reaction was higher for the catalysts prepared at low pH. (C) 2007 Elsevier B.V. All rights reserved.