y the rapid development of industry and new technologies, environmental pollution leading to an increased threat of human health, particularly in recent years the amounts of heavy metal ions in the wastewater have been increased. Heavy metal contaminants present in wastewater from several industries such as metal industries (steel, iron), metal plating, mining operations, textile and dyeing, battery, etc. Heavy metals are not biodegradable, hence have tendency to accumulation in the body of organisms that are causing disease and abnormalities. Removal of heavy metal ions doing in various ways, including physical and chemical adsorption methods. The chemical adsorption method, is a simple method to remove heavy metals from aqueous solutions that can be doing by polymer containing functionalized groups. In this investigation, Firstly nylon 66 nanofibrous Membranes have been produced with a thickness of 110 micrometers, average diameter of the nanofibers 287 nm and the electrospinning time 16 hours. Then the nanofiber membranes functionalized by trimercaptopropyltrimethoxysilane(TMPTMS) by sol-gel method. Two metal, cadmium and nickel, which are harmful heavy metals are chosen. The effect of filtration process parameters such as initial concentration of metal solution, pH of solution and pressure, and amount of functionalizer(TMPTMS) on the adsorption was studied. In surveying of filtration process parameters, the results showed that metal ion rejection increased by increasing the pH of solution and decreased by increasing initial concentration of effluent, and by increasing pressure the metal ion rejection initially increased and then decreased. By increasing the amount of functionalizer removal efficiency increased. Maximum efficiency of absorption of cadmium and nickel, respectively, 93.0% and 97.6% of the polymer solution of 19% (w/w) of nylon 66 was prepared in formic acid / chloroform mixture (75:25 v/v) on carbon foam for 16 hours, applied voltage of 12.5 kV and feed rate 0.314 ml/h, take up velocity 65 rpm, in the cross-flow filtration system for initial concentration 20 ppm for an hour at a pressure level of 1.7 bar and at pH 7 and amount of functionalizer 2/5 ml was obtained. Filtering mechanism of the membrane is block the pores type and metal ion adsorption isotherm for nylon 66 nanofiber membrane was Freundlich. The maximum adsorption capacity of Cd and Ni by Freundlich model, respectively, 956 and 1269 mg/g was shown to have a high capacity to work. Keywords: heavy metals, electrospinning, trimercaptopropyltrimethoxysilane, sol-gel, cross-flow filtration