A novel Nano/submicrofiber catalyst was prepared via electrospinning technology from poly (vinyl pyrrolidone) (PVP) and nano-TiO2. First, nano-TiO2 particles were added into the mixture of ethanol and deionized water, the mass ratio of ethanol and deionized water was 1 : 1, the TiO2 suspension was obtained after 1 h with ultrasonic treatment and centrifugal effect, Then PVP was added into the above-mentioned suspension and the content of PVP in the sol was 28%. The TiO2/PVP solution was electrospun with different voltage. The effects of the content of TiO2 and electrospinning voltage on diameter of nano/submicrofiber were studied. The nano/submicrofiber catalyst was characterized by scanning electron microscopy, transmission electron microcopy, X-ray diffraction, and Fourier transform infrared. The results show that the diameter of nano/submicrofiber increases with an increase of the content of nano-TiO2 and decreases with the increase of electrospinning voltage. The analytical result showed that the nano-TiO2 particles were well dispersed in the matrix of PVP, moreover, the crystal type of nano-TiO2 was a mixture of anatase and rutile and the diameter of nano-TiO2 particles in the nano/submicrofiber is in the range of 2060 nm and the nano-TiO2 particle was monodisperse, and the nano-TiO2 particle and PVP molecule was connected by a hydrogen bonding. This nano/submicrofiber catalyst has a high efficiency on degradation on CH2O. 56.8 percent of CH2O was degraded under ultraviolet radiation in 80 min when the content of nano-TiO2 is 20% in nano/submicrofibers. (c) 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012