A highly visible-light responsive AgI-TiO2/PAN had been successfully synthesized by the electrospinning technique, hydrogenation reduction, solvothermal synthesis, and gas/solid oxidation. The component and morphology of the as-prepared catalysts were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS), and Fourier transform infrared spectroscopy (FUR). In the degradation experiments, the as-prepared AgI-TiO2/PAN showed a highly photocatalytic activity in degrading methyl orange (MO) under visible light irradiation and the AgI content had a strong effect in their photocatalytic activity. Moreover, the degradation efficiency of MO over AgI-TiO2/PAN was much higher as compared to that of pure PAN, AgI/PAN and TiO2/PAN, which was attributed to the synergistic effect between AgI and TiO2. Besides, AgI-TiO2/PAN had an excellent stability in the cycling tests due to the intimate connect and stable heterostructure of AgI-TiO2. It's astonished to find that the application of PAN nanofibers, which presented in membranous form, made it easy separate the catalysts from an aqueous solution without any loss. (C) 2016 Elsevier Ltd. All rights reserved.