A heterogeneous catalyst was prepared by direct physical encapsulation of nickel Schiff- base complex into the silicon dioxide matrix via sol-gel method. The compounds were characterized by FT-IR, SEM, TEM, XRD, CHNS, and AAS. The catalytic performance in the alcohols and thiols oxidation was investigated in the presence of H2O2 (10 mmol, 30%) as oxidant. After five recycle runs, the catalyst showed 13% reduction in activity with slightly ...