A sol-gel process in reverse microemulsion combined with solvent-thermal technique was developed for synthesizing a series of nanomagnets supported TiO2 (TiO2/NMs) photocatalysts in this study. The structure of TiO2/NMs photocatalysts was characterized by Fourier transform infrared (FTIR),TG-DSC, Xray diffraction (XRD), Raman spectrometry, TEM, BET, and VSM. The influence of CoFe2O4 dosage on the photocatalytic activity and magnetism of TiO2/NMs photocatalysts was investigated. The results showed that nanosized anatase TiO2 were uniformly coated on spinel CoFe2O4 in the prepared TiO2/NMs photocatalysts. They possessed typical ferromagnetic hysteresis and performed better photocatalytic activity in degradation of methylene blue than TiO2 prepared by the same method. The existence of CoFe2O4 nanomagnets played an important role on the crystalline grain size of TiO2 and the specific surface area of the prepared TiO2/NMs photocatalysts, thus had an important influence on its photocatalytic performance and magnetism. The photocatalytic performance of TiO2/NMs photocatalysts is related to their specific surface area, crystalline grain sizes of TiO2 and particle size, as well as the doping effect of Fe3+. The highest photocatalytic activity in degradation of methylene blue for TiO2/NMs photocatalysts at the CoFe2O4 content of 20 wt.% was achieved, with k(p) 28.32% higher than that of pure TiO2 photocatalyst. Moreover, the experiments on recycled use of TiO2/NMs photocatalyst demonstrated a good repeatability of the photocatalytic activity. (c) 2009 Elsevier B.V. All rights reserved.