Nano-F/Zn/TiO2 particles were prepared by sol-gel method using NH4F and Zn(NO3)2 as dopants. The photocatalytic degradation of methylene blue in aqueous solution as simulated wastewater was used to evaluate their photocatalytic activities. The powders were characterized by energy dispersion X-ray spectrum (EDS), X-ray diffraction (XRD) transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area analysis. The results showed that F and Zn elements were doped into TiO2. The appropriate codoping amount for F and Zn were n(F)/n(TiO2)=2% and n(Zn)/n(TiO2)=3% respectively. The degradation rate of methylene blue at 1 h was improved from 73.2% to 86.2% by using F/Zn/TiO2 as photocatalyst.