Using sol-gel method, the iron-containing nanocomposites with the ferric citrate as iron raw were synthesized. The clear sols were gelated at room temperature and then treated at 60 _oC in vacuum to get dry gels which were characterized by thermogravimetricSanalysis (TG). Finally, mesoporous Fe₂O₃/SiO₂ nanoparticles were obtained by the calciner at 400 _oC for 3h. The structural properties of synthesized particles were investigated by X-ray diffraction (XRD), N₂ adsorption-desorptionStechnique, transmission electron microscopy (TEM), Fourier-transform IR spectroscopy (FT-IR), and Temperature programmed reduction (H₂-TPR), which revealed that the iron active centers were successfully incorporated into the silica framework with spherical particles size about 50 nm and a average pore diameter of 30-45 ?. The catalytic activity of nanocatalysts had been tested in the synthesis diphenylmethane by Friedel-Crafts alkylation reaction. It found that the catalysts exhibited an excellent activity with 100% conversion of benzyl chloride and relatively higher selectivity to diphenylmethane, and could be reusedSmultiple times.