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Synthesis of [Si]-MCM-41 from TEOS and water glass: the water glass-enhanced condensation of TEOS under alkaline conditions

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Abstract

Mesoporous [Si]-MCM-41 molecular sieve systems have been fabricated by aging silica gels in CTAB both at RT and under hydrothermal conditions with or without stirring. For the synthesis involving water glass as a SiO2 source, optimal conditions (100 °C, pH 10, crystallization time 2–3 days) gave reproducible, highly ordered [Si]-MCM-41 materials in multi gram scale with high lattice parameter values and BET surface areas. The synthesis with TEOS as silica source produced an inferior quality material. A novel synthesis route involving the use of mixtures of the two precursors gave [Si]-MCM-41 with improved structural (XRD) and microstructural (HRTEM) long-range order. Addition of small amounts of water glass to a TEOS-based synthesis gel under stirred conditions produced [Si]-MCM-41 with excellent mesoporosity, long-range microstructural order, XRD and S BET properties. These properties are reminiscent of those for materials obtained from water glass as a sole SiO2 source. The advantage of this route is that it gave high-quality materials at relatively lower temperatures (80 °C) and shorter crystallization times (6 h) after 21 h aging at RT. The variation of the XRD d 100 peak position, BET and HRTEM properties with [TEOS]/[water glass] ratio revealed that a ratio = 3.95 gave optimal production of the highly ordered materials. The data suggests that water glass acts as a structure-directing agent for the TEOS and is incorporated into the final structure.

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Acknowledgments

The authors would like to thank Professor A. K. Datye, Mangesh Bore and Kelvin Lester (University of New Mexico, USA) for their kind assistance with HRTEM imaging and the time spent in their laboratory as a doctoral student. Financial support from the NRF (National Research Foundation) and the granting of a PhD study leave by the University of Limpopo are acknowledged.

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Authors and Affiliations

  1. Department of Chemistry, University of Limpopo, P/Bag X1106, Sovenga, Polokwane, 0727, Republic of South Africa

    M. P. Mokhonoana

  2. Molecular Sciences Institute, School of Chemistry, University of the Witwatersrand, P/Bag 3, WITS, Johannesburg, 2050, Republic of South Africa

    M. P. Mokhonoana & N. J. Coville

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  1. M. P. Mokhonoana
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  2. N. J. Coville
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Correspondence to N. J. Coville.

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Mokhonoana, M.P., Coville, N.J. Synthesis of [Si]-MCM-41 from TEOS and water glass: the water glass-enhanced condensation of TEOS under alkaline conditions. J Sol-Gel Sci Technol 54, 83–92 (2010). https://doi.org/10.1007/s10971-010-2161-5

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