Bimetallic iron and vanadium incorporated SBA-15 molecular sieves (FVS) has been hydrothermally synthesized. XRD, TEM and N-2 adsorption-desorption results show that the FVS catalyst has a 2D P6mm hexagonal structure. ESR and UV-vis spectroscopic investigations suggested that the tetrahedrally coordinated iron and. vanadium species incorporated within the silica framework. The FVS catalyst exhibited high activity toward hydroxylation of benzene with molecular oxygen, over which the yield of phenol reaches 14.5%.