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Issue 9, 2014
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One-step synthesis of a highly homogeneous SBA–NHC hybrid material: en route to single-site NHC–metal heterogeneous catalysts with high loadings

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Abstract

The one-step synthesis of a mesoporous silica of SBA type, functionalized with a 1-(2,6-diisopropylphenyl)-3-propyl-imidazolium (iPr2Ar-NHC-propyl) cation located in the pore channels, is described. This material was obtained by the direct hydrolysis and co-condensation of tetraethylorthosilicate (TEOS) and 1-(2,6-diisopropylphenyl)-3-[3-(triethoxysilyl)propyl]-imidazolium iodide in the presence of Pluronic P123 as a non-ionic structure-directing agent and aqueous HCl (37%) as an acid catalyst. Small-angle X-ray diffraction measurements, scanning and transmission electron microscopies, as well as dinitrogen sorption analyses revealed that the synthesized material is highly mesoporous with a 2D hexagonal arrangement of the porous network. 13C and 29Si CP-MAS NMR spectroscopy confirmed that the material contains intact iPr2Ar-NHC-propyl cations, which are covalently anchored via silicon atoms fused into the silica matrix. Moreover, comparison of the latter data with those of an analogous post-synthetic grafted SBA–NHC material allowed us to establish that, as expected, (i) it is most probably more homogeneous and (ii) it shows a more robust anchoring of the organic units. Finally, elemental mapping by energy dispersive X-ray spectroscopy in the scanning electron microscope demonstrated a very homogeneous distribution of the imidazolium units within the one-pot material, moreover with a high content. This study thus demonstrates that a relatively bulky and hydrophilic imidazolium unit can be directly co-condensed with TEOS in the presence of a structure-directing agent to provide in a single step a highly ordered and homogeneous mesoporous hybrid SBA–NHC material, possessing a significant number of cationic NHC sites.

Graphical abstract: One-step synthesis of a highly homogeneous SBA–NHC hybrid material: en route to single-site NHC–metal heterogeneous catalysts with high loadings

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Publication details

The article was received on 22 Oct 2013, accepted on 16 Dec 2013 and first published on 17 Dec 2013


Article type: Paper
DOI: 10.1039/C3DT52982G
Citation: Dalton Trans., 2014,43, 3722-3729
  • Open access: Creative Commons BY license
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    One-step synthesis of a highly homogeneous SBA–NHC hybrid material: en route to single-site NHC–metal heterogeneous catalysts with high loadings

    M. Rocquin, M. Henrion, M. Willinger, P. Bertani, M. J. Chetcuti, B. Louis and V. Ritleng, Dalton Trans., 2014, 43, 3722
    DOI: 10.1039/C3DT52982G

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