Mesoporous sulfated Al2O3-ZrO2 (MSAZ) catalysts with large surface areas and pore volumes after calcination at high temperature (650 degrees C) and with higher Al2O3 content than 20wt% were successfully prepared from a template of block copolymer (P84). The MSAZ catalysts were characterized by X-ray diffraction (XRD), N-2 adsorption, transmission electron microscopy (TEM), Al-27 magic-angle spinning nuclear magnetic resonance (MAS NMR), thermogravimetric analysis (TG-DTG), temperature-programmed desorption of ammonia (NH3-TPD) and infrared spectra (IR) of adsorbed pyridine. It is shown that the resulting mesostructured sulfated Al2O3-ZrO2 samples have a well-developed textural mesoporosity. The number of acid sites present on MSAZ catalysts is higher than that on conventional sulfated zirconia, and the former catalysts are more active than the latter one for various acid-catalyzed reactions.