Insoluble porous solid, macrocyclic 22-membered ring, 1-oxa-6,9,12,15,18-pentaaza-2,22-disilacyclododocosane polysiloxane ligand system has been prepared by the reaction of a macro-silane agent with tetraethylorthosilicate. The macro-silane agent was prepared by the reaction of imino-bis(N-2-aminoethylacetamide) ligand with 3-iodopropyltrimethoxysilane in 1:3 molar ratio. The new prepared polysiloxane system exhibits variable potentials for the extraction of metal ions (Fe3+, Co2+, Ni2+, Cu2+, Zn2+, Ag+, Cd2+, Hg2+, and Pb2+) from aqueous solutions. The ligand system shows high capacity to extract silver, lead, and mercury. Chemisorption of the metal ions by the ligand system at the optimum conditions was found in the order Ag + > Pb2+ > Hg2+ > Cu2+ > Ni2+ > Fe3+ > Co2+ > Cd2+ > Zn2+.
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