Triple layer membranes of different proportions were prepared by using the combination of electrospinning and dry-wet phase inversion technique. The polymer solution of Nylon/PEG was prepared and poured over the electrospun polyacrylonitrile (PAN) nanofibers. Thus, prepared triple layer membranes were characterized by optical microscope, scanning electron microscope, porosimeter, X-ray diffraction, and thermogravimetric analyzer to study the morphology, pore size distribution, crystallinity, and degradation properties respectively. The performance of the triple layer membranes was evaluated by pure water flux and filtration efficiency. The results revealed that the triple layer membrane with the proportion of 60/40 (Nylon/PEG) has optimal pure water flux and higher filtration efficiency than the other prepared triple layer membranes.