Composite nanofibers containing polyacrylonitrile and natural clay particles were fabricated and investigated for the removal of Pb(II), Cu(II) and Zn(II) from aqueous solutions. The adsorption behavior of Pb(II), Cu(II) and Zn(II) can be well described by the Langmuir adsorption model and high loading capacities at pH 7 were obtained. The kinetics of the adsorption process showed that equilibrium was attained after 60 min and the experimental data followed a pseudo-first-order model. The nanocomposites were also tested for photocatalytic degradation of Monocrotophos pesticides in which high degradation efficiency (>90%) was obtained in less than 60 min.