Fibrous mats of polymer/clay were obtained by electrospinning method, and their capacity for heavy metals removal from water was evaluated. Four different fibrous mats were prepared from a corresponding polymer/clay solutions. The precursor materials employed were poly-epsilon-caprolactone, polyvinyl alcohol polymers, kaolin, and metakaolin clays. Raw materials and the prepared fiber mats characterization were carried out using scanning electron microscopy, Fourier transformed infrared spectroscopy, X-ray diffraction, termogravimetric analysis, differential thermal analysis, and differential scanning calorimetry. Elemental composition of the materials was obtained using energydispersive X-ray spectroscopy. The environmental applications of polymer/clay materials were tested for water treatment by heavy metals (cadmium (Cd+2), chromium (Cr+3), copper (Cu+2), and lead (Pb+2)) sorption. Kinetic adsorption studies were conducted employing heavy metal solutions with initial concentration of 200 mg/L, and the amount of heavy metal adsorbed and kinetics parameters was determined using inductively coupled plasma-optical emission spectroscopy (ICP-OES). According to the kinetic data, the adsorption process of Cd+2, Cr+3, Cu+2, and Pb+2 onto polymer/clay is favorable for the prepared materials and they follow a pseudo-first-order model according to the kinetic analysis. Additionally, the intraparticle diffusion was evaluated by applying the Morris andWeber model; in order to investigate the contribution of film resistance to the kinetics of the heavy metals adsorption, the adsorption kinetic data was further analyzed by Boyd's film-diffusion model.