Graphic carbon nitride polymer was modified with transition bimetals compounds by impregnation ofpre-prepared g-C3N4 in aqueous solution of ammonium molybdate and vanadate. The prepared hybridmaterial was characterized by XRD, SEM, TEM, FT-IR, XPS and N2 adsorption–desorption techniques todetermine its surface morphology, composition and structure. The results revealed that VOx-MoOy singlemolecular layer incorporated into g-C3N4 molecule framework by interaction between host and guestwas fabricated. The hybrid composite was employed as catalyst for styrene oxidation to benzaldehydeusing molecular oxygen as oxidant. The results indicated that the composite was highly active and selectivefor styrene oxidation, giving TON 458.8 mol/mol(Mo+V) and 96.7% selectivity to benzaldehyde. Thecorrelation between high activity and surface properties the catalyst was explored.