Using post grafting method, two hybrids composite materials were prepared by anchoring Nickel and Zinc Schiff base complexes onto amino-modified MCM- 41(Ni-MCM-41 and Zn-MCM-41). The prepared catalysts have been characterized by FT-IR spectroscopy, thermogravimetric analysis, and transmission electron microscopy, powder X-ray diffraction and N2 adsorption– desorption isotherms. The catalysts showed excellent catalytic efficiency in oxidation reaction of sulfides to sulfoxides and oxidative coupling of thiols to their corresponding disulfides using urea hydrogen peroxide as oxidant under mild reaction conditions. The supported Schiff base complexes can be recovered easily and reused many times without significant loss in catalytic activity and selectivity.