Abstarct: Recently, polysilesesquioxane have been attracted to researchers because of their unique properties. Their properties include high surface tension and hydrophobicity, high flexibility at ambient temperature, good biocompatibility and good glass transition temperature. In the present study, a kind of polysilesesquioxane was prepared using sol-gel method using 3-amino propyltriethoxy silane (APTES) and methyltrimethoxy silane (MTMS). Then, it reacted with hydroxyl benzyl aldehyde in one step. Subsequently, the molybdenum complex was immobilized on it and a heterogeneous Mo-PS catalyst. FT-IR, TG/DTA, SEM, XRD, CHN and ICP techniques was utilized, in order to confirm each synthesis step having been successfully done, and also to study the characteristics of compounds. This catalyst was found as an efficient catalyst for epoxidation of wide variety of alkenes, including aromatic and aliphatic alkeny using tert-butyl hydroperoxide as oxidant. This new heterogenized catalyst could be recovered and reused four consecutive and only 5% of its catalytic activity fell.