A thiol-functionalized layered magnesium phyllosilicate material (called Mg-MTMS), prepared by a direct and cost-effective co-condensation synthesis, has been investigated as a high-capacity adsorbent for heavy metal ions. Structural characterization by powder X-ray diffraction, infrared spectroscopy, solid-state 13{sup left}C and 29{sup left}Si NMR spectroscopies, and elemental analyses confirms the smectite-type structure and the high organic moiety content of this material. Mg -MTMS was found to be highly effective for the adsorption of Hg(II), Pb(II), and Cd(II) ions, exhibiting unprecedented metal ion uptake capacities of 603,365, and 210 mg of metal/g of adsorbent, respectively. Mg-MTMS shows an equivalent affinity for the three metal ions, removing them from mixed metal solutions with an equation uptake capacity (～400 mg of metal/g of adsorbent). Metal-loaded Mg-MTMS can be regenerated by acid treatment without altering the adsorbent properties. The high effectiveness of Mg-MTMS for the capture of metal ions is attributed to both the high concentration of complexing thiol groups (6.4 mmol of SH/g of Mg-MTMS) and the expansion capability of the framework, which facilitates the accessibility of the binding sites.
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