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Synthèse, caractérisation et réactivité en milieu aqueux de matériaux à base de silice fonctionnalisée par des ligands dithiocarbamate et cyclame

Abstract : Dithiocarbamate- and cyclame-functionalized mesoporous silicas have been prepared and characterized. Their reactivity in aqueous medium has been investigated to evaluate their potential use as electrochemical sensors. A novel one-step route towards dithiocarbamate-silicas has been developed thanks to the original synthesis of siloxydithiocarbamate precursors. This is based on the direct grafting of the precursor onto the silica surface. Mesoporous silicas (ordered or not, i.e., K60, SBA15, MCM41) functionalized with dithiocarbamate moieties have thus been obtained. Analogous materials have also been prepared according to the sole two-step procedure available to date in the literature (reaction of CS2 onto an amino-silica). The interest of the proposed approach compared to the one previously reported is to access undamaged dithiocarbamate-modified silicas, free of remaining amino groups, displaying better efficiencies for Hg(II) uptake. Three cyclam derivatives bearing 1, 2 or 4 silylated arms have been grafted onto mesoporous silicas (K60 and SBA15). Increasing the silylation degree improves the material stability in aqueous medium without preventing the leaching of the organic moiety usually observed for amino-silicas. Higher stability of the material, poorer reactivity towards protons and Cu(II) binding have been noticed. Cu(II) uptake process seems to be rate-limited by the kinetics associated to complex formation rather than mass-transfer rates into the porous matrix. Incorporation of these materials into carbon paste electrodes has led to a selective amperometric sensor for Cu(II).
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Stéphanie Goubert-Renaudin. Synthèse, caractérisation et réactivité en milieu aqueux de matériaux à base de silice fonctionnalisée par des ligands dithiocarbamate et cyclame. Autre. Université Henri Poincaré - Nancy 1, 2007. Français. ⟨NNT : 2007NAN10127⟩. ⟨tel-01748258⟩

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