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Polyacrylonitrile (PAN) nanofibers were prepared by an electrospinning technique. PAN nanofibers were chemically modified with amidoxime groups. The titanium oxide (TiO2) was then introduced to amidoxime-modified PAN (OM-PAN), which was then used for the photodegradation of methylene blue in aqueous solution. The morphology and photodegradation study was investigated by using scanning electron microscopy (SEM) and UV-visible spectrophotometry, respectively. The SEM study showed the presence of TiO2 particles on the surface of OM-PAN nanofiber mat in agglomerated form and was confirmed by energy dispersive X-rays analysis. The photodegradation study of methylene blue showed that the dye degradation was increased as increased in the irradiation time. The effect of pH on degradation efficiency showed that with an increase in pH the degradation efficiency increases.