ABSTRACT A new hybrid cation exchange material PANI-Ti(IV) phosphosulphosalicylate was synthesized by intercalating polyaniline (PANI) into Ti(IV) phosphosulphosalicylate (Ti(IV) PSS) using sol-gel chemical route. Then, it is renewed into H+ form and used as an adsorbent for the removal of Pb(II) from aqueous solution. The morphology and structure properties of the as prepared hybrid cation exchange material were characterized by X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy (SEM), Brunauer-Emmett-Teller (BET), thermo gravimetric analysis (TGA-DTG), and Transmission Electron Microscopy (TEM). The sorption experiment for Pb(II) removal was performed using batch method. Dependence of adsorption on contact time, exchanger dose, Pb(II) initial concentration, pH, and temperature has been studied to achieve the optimum conditions. The adsorption isotherm, kinetics, and thermodynamics of PTPSS for Pb(II) were studied. The results of the above mentioned analyses show that the adsorption isotherm process of Pb(II) on PTPSS was closely related to Langmuir model (r2 > 0.998). The adsorption kinetic process fits well with the pseudo-second order equation. Thermodynamic studies suggested the spontaneous and exothermic nature of PTPSS system. The ion exchange adsorbent shows ion exchange capacity for Li+, Na+, and K+ ions have been found to be 1.75, 2.24, and 2.41 meq/g, respectively. Its selectivity was examined by achieving some important binary separations like Pb2+- Cd2+, Pb2+- Hg2+, Pb2+- Cu2+, Pb2+- Zn2+, Pb2+- Ni2+, and Pb2+- Fe3+ on its column. On the basis of distribution studies (Kd values), PTPSS was highly selective for Pb(II). Therefore, the hybrid cation exchange material PTPSS can be used as a potential ion exchange material for the selective separation of Pb(II) ion in environmental remediation.