The solid superacid S2O82-/TiO2 supported oil inesoporous MCM-41 was prepared by the liquid-phase precipitation, and the mechanism for the formation of superacid was suggested. The esterification reation of acetic acid and iso-amyl alcohol was selected as a probe reaction to test the catalytic performance. The optimum conditions for preparation of the catalyst were obtained as follows: molar ratio of Ti to Si was 1:1, concentration of (NH4)(2)S2O8 was 0.5 mol(.)L(-1), impregnation time was 5 h, calculations temperature and time were 550 degrees C and 4 h, respectively. The structure of the solid superacid was characterized by XRD, N-2 Adsorption/desorption and FTIR. The results showed that inesoporous structure of MCM-41was maintained in the catalyst system with a high BET surface area of 211 m(2.)g(-1) and better solid acidity.