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ZSR-P loaded nano-TiO 2 composite photocatalysts (TiO 2 /ZSR-P) have been prepared by the sol–gel method using the by-product Zr-containing silica residue (ZSR) as precursors during the production process of zirconium oxychloride, the structure and properties of TiO 2 /ZSR-P were characterized in this paper. The results showed that the TiO 2 /ZSR-P composite photocatalysts were characterized by the uniform loading of nano-TiO 2 on the surface of amorphous SiO 2 particles in ZSR-P. TiO 2 and SiO 2 were combined by forming -Ti-O-Si- bonds at the interface and the crystalline structure of TiO 2 powders was identified a mixed phase of anatase and rutile, its loading amount was 17.14%, the particle size raged from 7 to 12 nm. The degradation rate of TiO 2 /ZSR-P to the concentration of 5 ppm and 10 ppm methyl orange solution reached 99.52% and 100% respectively after 140 min of ultraviolet irradiation, and it still maintained stable performance after repetitive-use of the catalyst for 4 times. [ABSTRACT FROM AUTHOR]