Thermally stable mesostructured sulfated zirconia (MSZ) with a high surface area has been successfully prepared by a novel one-step synthetic method involving the alcohothermal processing of zirconium nitrate in the presence of ammonium sulfate. The MSZ samples were characterized using X-ray diffraction (XRD), N-2 adsorption measurements, thermal analysis (TG/DTA) and transmission electron microscopies (TEM). It is shown that the resulting mesostructured sulfated zirconia samples are tetragonal crystalline, which have a high specific surface area and a well-developed textural mesoporosity with narrow pore size distribution. Catalytic testing showed that the present mesostructured sulfated zirconia was much more active than conventional sulfated zirconia for n-butane isomerization.