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The influence of synthesis conditions, oligosaccharide additive and functional silane on the structure and composition of sol–gel silicas

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Abstract

In this work, the influence of different experimental conditions on the structure and composition of silicas was elucidated. Sol–gel synthesis of silicas was realized in the presence of silica precursors (tetraethyl orthosilicate and (3-chloropropyl)triethoxysilane) as well as the β-cyclodextrin additive at various molar ratios of initial reagents. In addition, the effect of temperature on hydrolysis and condensation of silicon alkoxides (in the presence or the absence of oligosaccharide) at room temperature, 70 °C and 150 °C (hydrothermal treatment) was compared. Synthesized sol–gel silicas with different surface groups were characterized by IR spectroscopy, SEM and chemical analyses, low-temperature adsorption–desorption of nitrogen, and thermogravimetry. Chemical immobilization of functional groups on the surface of silica materials was proved by IR spectroscopy. The content of oligosaccharide moieties introduced into silicas in the process of sol–gel synthesis was estimated by acid hydrolysis of surface groups to glucose and its subsequent spectrophotometric determination. Morphology investigation was performed by SEM technique. The porous structure of synthesized silicas was elucidated by low-temperature adsorption–desorption of nitrogen. Gas-phase adsorption and liquid sorption experiments were carried out to study the role of silica’s structure and composition on benzene and phenol uptake, respectively. Synthesized silicas with chloropropyl and oligosaccharide moieties demonstrate adsorption level performance of known samples and are expected to be promising for the treatment of aqueous solutions from aromatics.

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Acknowledgements

The data of this study corresponded in part at the International conference “Nanomaterials: Applications and Properties” (NAP-2013). The full research was presented at the International conference “Nanotechnology and Nanomaterials (NANO-2021)” and submitted as the research article to a special issue.

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  1. Chuiko Institute of Surface Chemistry of NAS of Ukraine, 17 General Naumov Str., Kiev, 03164, Ukraine

    Iryna M. Trofymchuk & Lyudmila A. Belyakova

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  1. Iryna M. Trofymchuk
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Trofymchuk, I.M., Belyakova, L.A. The influence of synthesis conditions, oligosaccharide additive and functional silane on the structure and composition of sol–gel silicas. Appl Nanosci 13, 5211–5230 (2023). https://doi.org/10.1007/s13204-022-02742-w

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