A series of novel photocatalysts, H3PW12O40-Y-TiO2 nanocomposites with different H3PW12O40 loading levels (10%-40%) were prepared by impregnation method. And the Y-TiO2 support, doped with yttrium, was synthesized via sol-gel technique. The prepared catalysts were characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), nitrogen adsorption-desorption analysis and scanning electron microscopy (SEM). The processes allowed obtaining Keggin structure and crystallized anatase with large BET surface area as well as uniform distribution. The effects of H3PW12O40 loadings, catalyst dose, initial pH and concentration of dye solution on the degradation kinetics of methyl orange under UV light (λ≥365 nm) were discussed. Kinetics studies showed that the photocatalytic degradation of methyl orange fitted the apparent first-order reaction. Methyl orange was totally degraded in 21 min under optimum conditions: 20% loading, 0.03 g dose and pH 1.0. The catalyst was stable and easily to be separated from reaction system for recovery. And the Y-TiO2 support, doped with yttrium, was integrated via sol-gel technique. The series of novel photocatalysts, H3PW12O40-Y-TiO2 nanocomposites with different H3PW12O40 loading levels (10% -40%) were prepared by impregnation method. prepared catalysts were characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), nitrogen adsorption-desorption analysis and scanning electron microscopy (SEM). The processes allowed obtaining Keggin structure and crystallized anatase with large BET surface The effects of H3PW12O40 loadings, catalyst dose, initial pH and concentration of dye solution on the degradation kinetics of methyl orange under UV light (λ ≧ 365 nm) were discussed. Kinetics studies showed that the photocatalytic degradation of methyl orange fitted the apparent first-order reaction. Methyl orange was totally degraded in 21 min under optimum conditions: 20% loading, 0.03 g dose and pH 1.0. st was stable and easily to be separated from reaction system for recovery.