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Issue 19, 2009
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Rapid microwave-assisted synthesis of benzene bridged periodic mesoporous organosilicas

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Following extended use in organic chemistry, microwave-assisted synthesis is gaining more importance in the field of inorganic chemistry, especially for the synthesis of nanoporous materials. It offers some major advantages such as a significant shortening of the synthesis time and an improved promotion of nucleation. In the research here reported, microwave technology is applied for the synthesis of benzene bridged PMOs (periodic mesoporous organosilicas). PMOs are one of the latest innovations in the field of hybrid ordered mesoporous materials and have attracted much attention because of their feasibility in electronics, catalysis, separation and sorption applications. The different synthesis steps (stirring, aging and extraction) of the classical PMO synthesis are replaced by microwave-assisted synthesis steps. The characteristics of the as-synthesized materials are evaluated by X-ray diffraction, N2-sorption, thermogravimetric analysis, scanning- and transmission electron microscopy. The microwave-assisted synthesis drastically reduces the synthesis time by more than 40 hours without any loss in structural properties, such as mesoscale and molecular ordering. The porosity of the PMO materials has even been improved by more than 25%. Moreover, the number of handling/transfer steps and amounts of chemicals and waste are drastically reduced. The study also shows that there is a clear time (1 to 3 hours) and temperature frame (373 K to 403 K) wherein synthesis of benzene bridged PMO is optimal. In conclusion, the microwave-assisted synthesis pathway allows an improved material to be obtained in a more economical way i.e. a much shorter time with fewer chemicals and less waste.

Graphical abstract: Rapid microwave-assisted synthesis of benzene bridged periodic mesoporous organosilicas

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Publication details

The article was received on 20 Nov 2008, accepted on 10 Feb 2009 and first published on 17 Mar 2009

Article type: Paper
DOI: 10.1039/B820792E
J. Mater. Chem., 2009,19, 3042-3048

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    Rapid microwave-assisted synthesis of benzene bridged periodic mesoporous organosilicas

    G. Smeulders, V. Meynen, G. Van Baelen, M. Mertens, O. I. Lebedev, G. Van Tendeloo, B. U. W. Maes and P. Cool, J. Mater. Chem., 2009, 19, 3042
    DOI: 10.1039/B820792E

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