Several physicochemical techniques have been widely studied for heavy metals removal despite most of them are associated with challenges of higher cost, accessibility, and complex technical feasibility. In this study, nano-sorbent materials were developed from a naturally available clay matrices and its heavy metals (Cu2+ and Pb2+) removal capacity was tested at its pristine and iron impregnated form. Both top to down and borohydride reduction methods were used to produce the nano-sorbents. The nano-sorbents were characterized by XRD, XRF, SEM, FTIR, BET, and TGA/DGA. The sorption was studied in batch experiments. The surface area, pore-volume, and pore diameter of nano-clay were found 43.49 m2/g, 0.104 cm3/g, and 2.81 nm, respectively while iron impregnated nano-clay has shown a surface area (73.11 m2/g), pore-volume (0.153 m3/g), and pore diameter (3.83 nm). Both nanoparticles have shown a mesoporous nature. The highest Cu2+ and Pb2+ removal capacity of nano-clay was 99.2% (~11.9 mg/g) and 99.6% (~11.95 mg/g), respectively. Whereas, the iron impregnated nano-clay has achieved the highest Cu2+ and Pb2+ removal efficiency 99.8% (~11.97 mg/g) and 99.7% (11.96 mg/g), respectively. The highest Cu2+ adsorption efficiency of iron impregnated nanoclay was achieved at pH 5.0, adsorbent dose 0.83 g/L, contact time 150 minutes, and Cu2+ initial concentration 4 ppm while its highest Pb2+ adsorption activity was achieved at pH 5.0, contact time (90 minutes), Pb2+ initial concentration (6 ppm), and the adsorbent dose (0.67 g/L). Whereas, the Cu2+ adsorption using nano-clay was highest at pH 5.0, contact time (180 minutes), adsorbent dose (1.0 g/L), and Cu2+ initial concentration (2 ppm). While, pH 5.0, contact time (90 minutes), adsorbent dose (0.83 g/L), and Pb2+ initial concentration (4 ppm) was found to the conditions of highest Pb2+ removal. In all cases, the pseudo-second-order kinetics indicated the presence of chemisorption. Langmuir adsorption characteristics has been reflected on Pb2+ and Cu2+ removal activities of the nanoclay and iron impregnated nanoclay, respectively. Whereas, Freundlich isotherm model was better fitted for Cu2+ adsorption activity of the nanoclay. The −ΔG (<−20 KJ/mol), + ΔH°, and + ΔS° have shown a spontaneous and endothermic adsorption activity with a high level of adsorbents disorder. In general, the result of iron impregnated nano-clay has shown a promising result for the removal of Cu2+ and Pb2+ aqueous solution.