Nanocomposites in the form of continuous and aligned polyvinyl alcohol (PVA) nanofibers have been obtained by the electrospinning process. These fibers were used as matrix for hydroxyapatite (HA). PVA and PVA/HA nanofibers were fabricated and crosslinked with glutaraldehyde (GA). The hybrid of polymer with ceramics (HA) shows good properties of large surface area and good porosity that were demonstrated by different characterization techniques such as FTIR, SEM, XRD and EDX which illustrate the ratio of HA. The prepared nanofibrous membranes are used for removal of Zn2+ from simulated water. The potential of these synthesized sorbents to remove Zn2+ ions from aqueous solutions was investigated in batch experiments, where several parameters such as the sorbate/sorbent’s contact time, initial Zn2+ ions concentration and sorbent dosage were investigated. The equilibrium concentration of Zn2+ ions was identified by the atomic absorption spectrophotometry and the adsorption process was studied by the isotherm models such as Langmuir, Freundlich and Temkin. The Zn2+ adsorption process for PVA and PVA/HA nanofibrous membranes was fitted to Langmuir and Freundlich isotherm models respectively.