This work aims at the preparation and characterization of dual-layer (DL) nano-fibrous mat (NFM) of hydrophobic and mechanical stable polyacrylonitrile (PAN) nano-fibers (NFs), as a supporter, and polyamide 6 (PA)/chitosan (Ch) NFs as a top hydrophilic coating layer. PAN and PA fibers, as residual wastes from textile processes, were collected and dissolved in their proper solvents. PAN was electro-spuned under certain conditions of electro-spinning (voltage, flow rate, and distance between spinneret and collector) to obtain PAN-NFM. Different ratios of PA/Ch composite were prepared and then electro-spun above the PAN-NFM that was previously prepared to obtain hydrophobic/hydrophilic functional dual-layer nano-fibrous membrane (DLNFM). The efficiency of the prepared DLNFM for capturing dye residues and heavy metals from wastewater was investigated. The viscosities of the prepared composite solutions were measured. The prepared dual-layer nano-fiber membranes (DLNFMs) were chemically and physically characterized by Fourier transform infrared spectroscopy, scanning electron microscope, X-ray diffraction, and thermogravimetric analyzer. The potential of the prepared mats for the adsorption of some heavy metal ions, i.e., Cu, Cr, and Pb cations in addition to dyes from wastewater was evaluated. The effect of using different concentrations of PA/Ch composite as well as the thickness of the obtained DLNFM on the filtration efficiency was studied. The results of this study show the success of functional DLNFM in dye and heavy metal removal. The maximum removal efficiency of acid dyes was reached to 73.4 % and of reactive dye was approximately 61 % for PAN/PA-1.25%Ch DLNFM after 3 days at room temperature. The removal efficiency percent of heavy metal ions reached to 54 % by DLNFM. Additionally, the results showed that 0.08 mm is the ideal thickness for maximum absorption capacity. This value is correlated with the membrane's highest Ch percentage, which is (PAN/PA-1.25%Ch). Furthermore, the results demonstrate that the presence of the Ch polymer strengthened the produced bi-layered membrane to achieve the highest thermal stability when compared to the other nano-fibrous membranes (NFMs), with the breakdown temperature of the Ch functionalized dual-layer membranes (DLMs) reaching approximately 617 °C and a maximum weight loss of 60 %.