Hybrid nanofibers based on ZnO loaded activated carbon nanofibers (ZnO-ACNFs) are proposed here for the elimination of hazardous lead from aqueous solutions. The prepared ZnO nanoscale material was loaded into the polyacrylonitrile nanofibers (PAN NFs) which were later carbonized by using a novel method named as a plate-sandwich method. The Synthesized nanofibrous composite was characterized by SEM, TEM, EDX, FTIR and XRD techniques to analyze its chemical and morphological properties. Moreover, the nanocomposite was efficaciously applied for the lead (Pb2+) ions removal from wastewater and simulated water through continuous filtration and batch filtration. The ZnO-ACNFs membrane showed outstanding results in adsorptive removal, giving adsorption capacity of 92.59 mg/g within the contact time of 45 min. Compared to their counterparts (ZnO and CNFs), the hybrid ZnO-ACNFs showed excellent performance in removing toxic lead.