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Covalent grafting of organoalkoxysilanes on silica surfaces in water-rich medium as evidenced by 29Si NMR


This paper addresses two questions related to functionalization of silica particles: (1) is the grafting of hydrophobic organoalkoxysilanes on a silica surface possible in water-rich medium and (2) how to prove the formation of covalent bonds with the surface? Trimethylethoxysilane, dimethyldiethoxysilane and methyltriethoxysilane have been reacted with precipitated silica in water-rich medium (water/ethanol 25/75 v/v) and 29Si MAS NMR was used to answer both questions: 29Si chemical shift values of the organosilicon units in the case of trimethylethoxysilane and dimethyldiethoxysilane clearly distinguished between self-condensation reactions and surface reactions through covalent bonds.

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The authors are grateful to Rhodia Recherche for their financial support, Dr A. Pottier for her interest with this work, J. Maquet for assistance in solid state NMR and M-N. Rager in solution-state NMR.

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Correspondence to Florence Babonneau.

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de Monredon–Senani, S., Bonhomme, C., Ribot, F. et al. Covalent grafting of organoalkoxysilanes on silica surfaces in water-rich medium as evidenced by 29Si NMR. J Sol-Gel Sci Technol 50, 152–157 (2009).

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