The synthesis through click chemistry of triethoxysilylated cyclen derivative-based ligands is described. Different methods were used such as the copper catalyzed Huisgen's reaction, or thiol–ene reaction for the functionalization of the cyclen scaffold with azidopropyltriethoxysilane or mercaptopropyltriethoxysilane, respectively. These ligands were then grafted on magnetic mesoporous silica nanoparticles (MMSN) for extraction and separation of Ni(II) and Co(II) metal ions from model solutions. The bare and ligand-modified MMSN materials revealed high adsorption capacity (1.0–2.13 mmol g−1) and quick adsorption kinetics, achieving over 80% of the total capacity in 1–2 hours.
