Abstract
In-situ liquid-state 29Si nuclear magnetic resonance was used to investigate the temporal concentration changes during ammonia-catalyzed initial hydrolysis of tetraethyl orthosilicate in different solvents (methanol, ethanol, n-propanol, iso-propanol and n-butanol). Dynamic light scattering was employed to monitor simultaneous changes in the average diameter of silica particles and atomic force microscopy was used to image the particles within this time frame. Solvent effects on initial hydrolysis kinetics, size and polydispersity of silica particles were discussed in terms of polarity and hydrogen-bonding characteristics of the solvents. Initial hydrolysis rate and average particle size increased with molecular weight of the primary alcohols. In comparison, lower hydrolysis rate and larger particle size were obtained in the secondary alcohol. Exceptionally, reactions in methanol exhibited the highest hydrolysis rate and the smallest particle size. Ultimately, our investigation elaborated, and hence confirmed, the influences of chemical structure and nature of the solvent on the formation and growth of the silica particles under applied conditions.
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Financial support from the Scientific and Technical Research Council of Turkey (TUBITAK) under contact number 109M073 is gratefully acknowledged. The authors wish to acknowledge Burçin Yıldız for NMR measurements and fruitful discussions.
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Malay, O., Yilgor, I. & Menceloglu, Y.Z. Effects of solvent on TEOS hydrolysis kinetics and silica particle size under basic conditions. J Sol-Gel Sci Technol 67, 351–361 (2013). https://doi.org/10.1007/s10971-013-3088-4
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DOI: https://doi.org/10.1007/s10971-013-3088-4