The purpose of this work was to prepare a new Ni–carboxamide complex supported on CoFe2O4 nanoparticles (CoFe2O4/SiO2–NH2@carboxamide–Ni). The carboxamide host material unit generated cavities that stabilized the nickel nanoparticles effectively and prevented the aggregation and separation of these particles on the surface. This compound was appropriately characterized using FT-IR spectroscopy, FE-SEM, ICP-OES, EDX, XRD, TGA analysis, VSM, and X-ray atomic mapping. The catalytic oxidation of sulfides and oxidative coupling of thiols in the presence of the designed catalyst was explored as a highly selective catalyst using hydrogen peroxide (H2O2) as a green oxidant. The easy separation, simple workup, excellent stability of the nanocatalyst, short reaction times, non-explosive materials as well as appropriate yields of the products are some outstanding advantages of this protocol