In the present work, a novel hybrid ion-exchange material was synthesized by a sol−gel route, by treating titanium tetrachloride with claw-type amino tris(methylenephosphonic acid) (ATMP) to give titanium amino tris(methylenephosphonic acid) (Ti-ATMP). Ti-ATMP was characterized by elemental analysis (ICP-AES and C, H, N analysis), spectral analysis (FTIR), thermal analysis (TGA), XRD, SEM, and EDX spectroscopy, including physicochemical and ion-exchange characteristics. The equilibrium exchange of transition-metal ions (viz., Cu 2+ , Ni 2+ , Co 2+ Zn 2+ ) and heavy-metal ions (viz., Pb 2+ ,Cd 2+ , Hg 2+ ) with the H + ions contained in ATMP was studied at constant ionic strength and varying temperatures, and various thermodynamic parameters such as the equilibrium constant (K), standard Gibbs free energy (ΔG°), enthalpy (ΔH°), and entropy (ΔS°) were evaluated. The Nernst−Planck equation was used to study the ion-exchange kinetics, and various kinetic parameters, namely, the self-diffusion coefficient (D 0 ), energy of activation (E a ), and entropy of activation (ΔS*), were evaluated under conditions favoring a particle-diffusion-controlled mechanism. Metal-ion adsorptions with variations in concentration and temperature were studied using the Langmuir and Freundlich adsorption isotherms. The distribution coefficient (K d ) and breakthrough capacity (BTC) values for transition-and heavy-metal ions were determined. Based on K d (mL•g −1 ), the selectivity order for metal ions toward Ti-ATMP was found to be Cu 2+ (19820) > Zn 2+ (3280) > Co 2+ (2630) > Ni 2+ (2390) among transition-metal ions and Pb 2+ (3590) > Cd 2+ (2340) > Hg 2+ (610) among the heavy-metal ions. The elution behavior of these metal ions was studied using different acids and electrolytes. A study on regeneration and reuse of the ion exchanger Ti-ATMP shows that it is effective up to five cycles without much decline in performance, which indicates that Ti-ATMP has good potential for use as a cation exchanger.