A series of sulfated silica-doped tin oxides with large surface areas (113-188 m(2)/g) have been successfully prepared from hydrothermal synthesis, followed by sulfation and calcination. These samples are characterized by XRD, FT-IR, TEM, nitrogen isotherms, and TG techniques, and obtained results indicate that the samples are composed of tetragonal nanocrystalline tin oxides and amorphous silica. Very interestingly, catalytic tests show that these sulfated silica-doped tin oxides are much more active than conventional sulfated tin oxides for transesterification of triacetin with methanol.