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A novel nanocomposite (N–TiO2-α-Am.Ph) was designed by surface functionalization of nano titanium oxide (N–TiO2) with α-aminophosphonates (α-Am.Ph). A study was aimed to explore and investigate the uptake properties of (N–TiO2-α-Am.Ph) for divalent Pb/Cu ions. The synthesized nanocomposite was characterized by FT-IR, TGA, XRD and HR-TEM analyses. The particle size range of N–TiO2-α-Am.Ph was identified between 75.35 and 153.55 nm. The adsorption characteristics of α-Aminophosphonates (α-Am.Ph) were confirmed to improve upon immobilization on the surface of N–TiO2 as monitored by diverse experimental controlling parameters. The collected results revealed that (N–TiO2-α-Am.Ph) exhibited optimum removal conditions of divalent Pb/Cu at pH 7.0 and reaction time at 60 min. Different models of adsorption isotherm and kinetics studies for the metal uptake were evaluated. The performance characteristics of (N–TiO2-α-Am.Ph) for remediation of divalent Pb/Cu ions from drinking water and industrial wastewater were successfully accomplished with 90–94% recovery using the micro-column system.