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Polyacrylamide zirconium (IV) iodate was synthesized using the sol–gel technique. The synthesis conditions such as reactant concentrations and temperature were changed to optimize the ion exchange properties of the hybrid organic–inorganic ion exchange material. Zirconium oxychloride (0.1 M) was added to 0.1 M potassium iodate in the presence of 0.4 M acrylamide and heated at 70 °C for 6 h to yield the polyacrylamide zirconium (IV) iodate with maximum capacity. The ion exchange capacity was found to be 3.27 meq/g for Pb(II). The hybrid material has been characterized on the basis of chemical composition FTIR, XRD, TGA-DTA, SEM and EDX studies. Sorption studies showed that the hybrid cation exchanger has a high selectivity to Pb(II) in comparison to other metal ions. Its selectivity was evaluated by performing some important binary separations like Hg(II)–Pb(II), Cu(II)–Pb(II), Ni(II)–Pb(II), Fe(III)–Pb(II) and Cd(II)–Pb(II). In addition, the selective separation of Pb(II) was also achieved from a synthetic mixture containing a large number of metal ions with a recovery of ∼98.5%. The proposed method was successfully applied for the selective removal of Pb(II) from wastewater samples.