In this study, the multi-walled carbon nanotubes were oxidized by m-chlorperbenzoic acid followed by the reaction with titanium n-butoxide and nickel nitrate to prepare Ni distributed CNT/TiO2 composite by a simple sol-gel method. The functional groups formed on the surface of MWCNTs were analyzed by Fourier transform infrared spectroscopy. The prepared Ni distributed CNT/TiO2 composite was characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and energy dispersive X-ray analysis. The photodegradation of methylene blue, methylene orange and rhodamine B solution under UV irradiation was employed to test the photocatalytic activity of the Ni distributed CNT/TiO2 composite. According to the results, Ni distributed CNT/TiO2 composite showed very excellent photocatalytic activity to decompose MB, MO and Rh.B solutions, due to the electron absorption effect of MWCNTs and electron trapping effect of nickel.