MCM-48 were prepared using hexadecyl trimethyl ammonium bromide and TEOS and modified with N1-(3-trimethoxysilylpropyl) diethylenetriamine by post-synthesis method to develop efficient adsorbent for heavy metal adsorption. These materials were determined by X-ray diffraction, N2 adsorption–desorption measurement, and scanning electron microscopy. The results show that the modification of MCM-48 resulted in a decrease in the Brunauer–Emmett–Teller surface area and total pore volume. Batch adsorption technique in the single and multicomponent systems was used in this study. The experimental parameters’ influence was investigated, and the results indicated that amine-attached MCM-48 indicated higher adsorption efficiency for metal ions than MCM-48. Langmuir and Freundlich models modeled the equilibrium data in a single system, whereas two-component data fitted to the extended Langmuir model. The maximum adsorption capacity (qm, single system) of NH2-NH-NH-MCM-48 for cadmium and lead was 82.7 and 119.24 mg g−1, respectively. In both adsorption systems, the affinity of NH2-NH-NH-MCM-48 for cadmium was more significant than that for lead.

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