Poly(methyl methacrylate)-titania(PMMA-TiO 2) nanocomposites were synthesized from tetrabutyl titanate(TBT) and methyl methacrylate(MMA) by sol-gel process using methacryloyloxypropyl trimethoxy siliane(MPTMS) as coupling agent and dilute hydrochloric acid as catalyst. Reaction parameters affecting the character of the products, such as the concentration of HCl, amount of water and coupling agent were discussed. The results showed that considerable good product can be obtained when the concentration of HCl is (0.3±0.02) mol/L, n(TBT)∶n(H 2O)>5∶1 and n(MPTMS)/n(TBT)>1. The chemical structure of PMMA-TiO 2 was characterized by IR, TEM and TG/DTA.