Fe(III)meso-tetraphenylporphyrinated polyacrylonitrile fiber mat supported TiO 2 photocatalyst (PANC/ TiO 2 mat) was prepared via copolymerization and electrospinning. SEM images showed that well-defined fibers with diameters around 1.47 ± 0.26 μ m were fabricated from Fe(III)meso-tetraphenylporphyrin (FeTPP)-acrylonitrile copolymer (PANC) and TiO 2 mixture. The XRD characterizations demonstrated that the electrospinning process had no effect on the anatase structure of TiO 2 . The photocatalytic activity of the PANC/TiO 2 mat was examined for the photodegradation of methyl red in aqueous solution under the irradiation of visible light. The results showed that this PANC/TiO 2 fiber mat was very efficient for the photodegradation of methyl red, with a degradation percentage over 94%. It is worth noting that the PANC/TiO 2 mat could be easily recovered and reused 3 times without any destruction of fiber morphologies.