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Fe(III)meso-tetraphenylporphyrinated polyacrylonitrile fiber mat supported TiO2 photocatalyst (PANC/ TiO2 mat) was prepared via copolymerization and electrospinning. SEM images showed that well-defined fibers with diameters around 1.47 \pm 0.26 m m were fabricated from Fe(III)meso-tetraphenylporphyrin (FeTPP)-acrylonitrile copolymer (PANC) and TiO2 mixture. The XRD characterizations demonstrated that the electrospinning process had no effect on the anatase structure of TiO2. The photocatalytic activity of the PANC/TiO2 mat was examined for the photodegradation of methyl red in aqueous solution under the irradiation of visible light. The results showed that this PANC/TiO2 fiber mat was very efficient for the photodegradation of methyl red, with a degradation percentage over 94%. It is worth noting that the PANC/TiO2 mat could be easily recovered and reused 3 times without any destruction of fiber morphologies.