Advanced oxidation with Fenton catalyst is the most common method for removal azo dyes. However, it is difficult to recover the heterogeneous nanocatalyst of Fenton process. Thus, the catalyst based on nanofibers can be overcome the drawbacks of nano catalyst. In this study, PVA/Fe₂O₃ nanofibers were successfully synthesized by an electrospinning method. The morphologies and structures of the nanofibers were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM). PVA/Fe₂O₃ nanofibers were used for removal methyl orange (MO) in an aqueous solution. The concentrations of MO determined using a UV-Visible spectrophotometer. The effects of different variables on the removal efficiency of PVA/Fe₂O₃ nanofibers were studied, including initial concentration of amount of H₂O₂, and amount of nanofibers.