A collection of novel nanocomposites, including different loading levels of tin-derivative sandwich type polyoxometalate on Sm- doped TiO2 nanoparticles, were prepared by a simple imprgnation method. The catalysts were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), high resolution scanning electron microscope (SEM). The results showed that the sandwich type polyoxometalate was successfully loaded on the Sm-doped anatase phase TiO2 nanoparticles and particles ware relatively diameter 20-30 nm. The effects of operational parameters such as the amount of tin-derivative sandwich type polyoxometalate, catalysts dose, and initial pH solution on the degradation kinetics of dye under UV light (λ≥365 nm) were discussed. The kinetics studies showed that the of photocatalytic degradation of methyl orange fitted the apparen first-order reaction. The catalysts was stable and easily to be separated from reaction system for recovery.