A novel magnetically separable heterogeneous photocatalyst TiO2/CoFe2O4 nanofiber was prepared by sot-gel method and electrospinning technology, followed by heat treatment at 550 degrees C for 2 h. The phase structure, morphology and magnetic property of the composite nanofibers were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscope and vibrating sample magnetometer analysis. The photocatalytic studies of TiO2/CoFe2O4 fibers suggested that the presence of CoFe2O4 not only enhanced the absorbance of UV light, but also broadened the response region to visible light. The decolorizing efficiency of methylene blue (MB) solution reaches 95.87% over TiO2/CoFe2O4 nanofibers under 300 W Hg lamp after 5 h, which is close to that of Degussa P25. Furthermore, these fibers can be collected with a magnet for reuse and effectively avoid the secondary pollution of the treated water. (C) 2011 Elsevier Ltd. All rights reserved.