A series of sulfated zirconia nanoparticles (abbreviated to SZNP) with high surface area and mesostructure have been synthesized by using sulfate-contained anion surfactants (SDS and SCS) both as a template and a sulfating agent via one-step liquid-crystal template (LCT) route. In light of N-2 adsorption-desorption, XRD and FT-IR analyses, it can be concluded that SOS is in favor of the mesostructure formation as well as the inhibition of ZrO2 phase transformation from tetragonal to monoclinic with respect to SCS. The optimal molar ratio of Zr/S is 1:1, which lead to the largest BET surface area. It is well-demonstrated by FT-IR, NH3-TPD together with transesterification reaction that SO42- anion, originated from the hydrophilic moieties of templates, can be easily incorporated into ZrO2 to form SZNP with super acidity, and the formation mechanism is also illustrated. Catalytic data exhibiting the yield of fatty acid methyl ester (FAME) in transesterification of soybean oil with methanol is in the following order: SZNP(12-(550)-1.0) > SZNP(16-(550)-10) > TSZ((550)). (C) 2013 Published by Elsevier B.V.