Zirconia/surfactant composites were hydrothermally synthesized in aqueous sulfuric acid at 373 K using Zr(O-nPr)(4) as oxide precursor and hexadecyl-trimethyl-ammonium bromide as template. Mesostructural features similar to those of MCM-41 were detected by X-ray diffractometry, with d=4.6 nm. A sample obtained from a starting mixture with Zr:S:CTAB = 2:2:1 was stable enough for removal of occluded organics. After calcination at 813 K, the d-value was 3.6 nm, the surface area 200 m(2)/g, and the mean pore diameter estimated by the BJH method 2.2 nm. Extended X-ray absorption fine structure analysis suggests Zr to be in a short-range structure (<4 Angstrom) similar to that of Zr in monoclinic ZrO2. Scanning electron microscopy including energy dispersive X-ray analysis showed 1-5 mum sulfur-containing ZrO2 spheres. The material catalyzes the isomerization of n-butane to i-butane at 378 K with a steady activity in the order of magnitude of commercial sulfated ZrO2.