Abstract
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.
This is a preview of subscription content, access via your institution.




References
Liu X, Bordunov AV, Pohl CA (2006) J Chromatogr A 1119:128. doi:10.1016/j.chroma.2005.11.086
Guo RR, Ding MY (2007) Colloids Surf A Physicochem Eng Asp 292:153. doi:10.1016/j.colsurfa.2006.06.017
Trewyn BG, Slowing II, Giri S, Chen H-T, Giri S, Lin VS-Y (2007) Acc Chem Res 40:846. doi:10.1021/ar600032u
Lebret V, Raehm L, Durand J-O, Smaihi M, Werts MHV, Blanchard-Desce M, Methy-Gonnod D, Dubernet C (2008) J Sol-Gel Sci Technol 48:32
Price PM, Clark JH, Macquarrie DJ (2000) J Chem Soc, Dalton Trans 101. doi:10.1039/a905457j
Eaton P, Holmes P, Yarwood J (2000) Appl Spectrosc 54:508. doi:10.1366/0003702001949672
Collet J, Tharaud O, Chapoton A, Vuillaume D (2000) Appl Phys Lett 76:1941. doi:10.1063/1.126219
Moncada E, Quijada R, Retuert J (2007) Nanotechnology 18:335606. doi:10.1088/0957-4484/18/33/335606
Caravajal GS, Leyden DE, Quinting GR, Maciel GE (1988) Anal Chem 60:1776. doi:10.1021/ac00168a027
Sindorf DW, Maciel GE (1982) J Phys Chem 86:5208. doi:10.1021/j100223a029
Dkhissi A, Esteve A, Jeloaica L, Esteve D, Rouhani MD (2005) J Am Chem Soc 127:9776. doi:10.1021/ja040246u
Bourgeat-Lami E, Luna-Xavier J-L, Guyot A (2000) Mater Res Soc Symp Proc 628:CC3.5.1
Tao T, Maciel GE (2000) J Am Chem Soc 122:3118. doi:10.1021/ja991950r
Massiot D, Fayon F, Capron M, King I, LeCalvé S, Alonso B, Durand J-O, Bujoli B, Gan Z, Hoatson G (2002) Magn Reson Chem 40:70. doi:10.1002/mrc.984
Backer M, Grimmer A-R, Auner N, John P, Weis (1997) J Solid State NMR 9:241
Sutra P, Fajula F, Brunel D, Lentz P, Daelen G, Nagy JB (1999) Colloids Surf A 158:21
Sugahara Y, Okada S, Kuroda K, Kato C (1992) J Non-Cryst Solids 139:25. doi:10.1016/S0022-3093(05)80802-6
Babonneau F, Bois L, Livage J (1992) Mater Res Soc Symp Proc 271:237
Rankin SE, McCormick AV (1999) Magn Reson Chem 37:S27. doi:10.1002/(SICI)1097-458X(199912)37:13<S27::AID-MRC576>3.0.CO;2-5
Babonneau F (1994) Polyhedron 13:1123. doi:10.1016/S0277-5387(00)80249-1
Hasegawa I, Ishida M, Motojima S, Satokawa S (1994) Mater Res Soc Symp Proc 346:163
Acknowledgment
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.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
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). https://doi.org/10.1007/s10971-009-1920-7
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10971-009-1920-7