TiO2/Montmorillonite (TiO2/Mmt) composite was firstly prepared by the sol-gel method, then was put into the Fe(NO3)3-HNO3 system in order to form the nano-FeOOH/ TiO2/Mmt composite depending on the hydrolysis of Fe3+ through controlling pH, temperature and concentration.This sample could improve the photocatalysis effect in visible light.TEM result showed that the FeOOH/ TiO2 composite film is 10~40 nm thick, and TiO2 is anatase measured at 5~10 nm in size, on TiO2/Mmt surface the goethite nanofilm was formed which is measured at 10~30 nm in length, and 4 nm in width.Finally, the IR spectra of MO showed that the FeOOH/TiO2/Mmt/H2O2/UV system possesses the better photocatalytic activity than FeOOH/TiO2/Mmt/ H2O2/Visible light for the strong capability of oxidating benzene ring.