Abstract: A novel magnetic-nanometer titanium dioxide/silicon dioxide/ferrite nickel (TiO2/SiO2/NiFe2O4) composite photocatalyst where NiFe2O4 was coated by SiO2 as magnetic matrix，was prepared by means of the homogenous precipitation coating technique. Its optimal preparation conditions were obtained through adjustment of pH value，time of water-heat，temperature of water-heat，temperature of calcination，ratio of Ti/Ni，etc. The morphological structure of the photocatalyst particles was characterized with XRD and TEM analysis. The nanometer-TiO2 dispersed uniformly and enwrapped the SiO2/NiFe2O4 core to from composite particle with a size of 50～70 nm. The photocatalyst showed properties of absorptive wavelength red-shift by UV-vis analysis. The VSM analysis showed that the photocatalyst had good magnetic properties. The photo-catalytic reactivity of samples were evaluated by using methyl orange aqueous solution as simulated contaminants. The results showed that the photo-catalytic decolorization ratio was up to 98.6%.