Abstract
Molecular inclusion complexes between cyclodextrins and cyclic siloxanes were prepared and characterized via a combination of liquid and solid state NMR, FT-IR, TGA, powder X-ray diffraction, SEM–EDS and elemental analyses. The crystalline complexes adopted the channel-type conformation. Depending from the size of both the cyclic sugar cavity and the silicon guest, various yields (between 0 and 41%) and host–guest molar ratios (between 1:1 and 4:1) were obtained. α-cyclodextrin (α-CD) and β-cyclodextrin (β-CD) were observed to form crystalline inclusion complexes only with D3 (cyclic dimethyltrisiloxane) due to steric effects, whereas the larger γ-cyclodextrin (γ-CD) formed inclusion complexes both with D3, D4 (cyclic dimethyltetrasiloxane) and D5 (cyclic dimethylpentasiloxane). This study is believed to be the first step towards the selective removal of cyclic siloxanes impurities from commercial PDMS preparations.
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Acknowledgments
This work was generously supported by Dow Corning. The solid-state NMR measurements were carried out at the EPSRC solid-state NMR service in Durham (UK). The X-ray crystallography analyses were performed by the EPRSC X-ray crystallography service at the University of Southampton (UK). The elemental analyses were conducted by MEDAC LTD, Brunel Science Centre (UK) in duplicate formats.
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Abbate, V., Bassindale, A.R., Brandstadt, K.F. et al. Inclusion complexes between cyclic siloxanes and cyclodextrins: synthesis and characterization. J Incl Phenom Macrocycl Chem 74, 223–230 (2012). https://doi.org/10.1007/s10847-011-0103-7
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DOI: https://doi.org/10.1007/s10847-011-0103-7