In this study, an iron oxide/carbon nanofibers (Fe2O3/CNFs) composite was prepared by a combination of electrospinning and hydrothermal methods. The characterization of Fe2O3/CNFs was achieved via scanning electron microscopy (SEM), infrared spectroscopy (IR), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). It is shown that when the hydrothermal reaction time was 180 °C and the reaction time was 1 h, the Fe2O3 nanoparticle size was about 90 nm with uniform distribution. The photodegradation performance applied to decolorize methyl orange (MO) was investigated by forming a heterogeneous Fenton catalytic system with hydrogen peroxide. The reaction conditions for the degradation of MO were optimized with the decolorization rate up to more than 99% within 1 h, which can decompose the dyes in water effectively. The degradation process of MO by Fenton oxidation was analyzed by a UV-visible NIR spectrophotometer, and the reaction mechanism was speculated as well.
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