Journal of Inclusion Phenomena and Macrocyclic Chemistry

, Volume 75, Issue 3, pp 247–254

Vibrational dynamics and hydrogen bond properties of β-CD nanosponges: an FTIR-ATR, Raman and solid-state NMR spectroscopic study

  • F. Castiglione
  • V. Crupi
  • D. Majolino
  • A. Mele
  • W. Panzeri
  • B. Rossi
  • F. Trotta
  • V. Venuti
Original Article

DOI: 10.1007/s10847-012-0106-z

Cite this article as:
Castiglione, F., Crupi, V., Majolino, D. et al. J Incl Phenom Macrocycl Chem (2013) 75: 247. doi:10.1007/s10847-012-0106-z

Abstract

Cyclodextrin nanosponges (CDNS) are cross-linked polymers with remarkable inclusion/release properties. CDNS show swelling capability and a hydrophilicity/hydrophobicity balance that can be dramatically modified by the type and quantity of cross-linking agents. Here, we focus our attention on samples of β-cyclodextrin nanosponges (β-CDNS) obtained by reacting β-cyclodextrin (β-CD) with the cross-linking agent carbonyldiimidazole at different β-CD:cross-linking agent molar ratio. The vibrational properties of CDNS thus synthesized have been investigated by Fourier transform infrared spectroscopy in attenuated total reflectance geometry and Raman spectroscopy in the dry state at room temperature. The quantitative analysis of the O–H stretching region (3,000–3,800 cm−1) allowed us to obtain structural information on the role played by primary and secondary OH groups in the hydrogen bond network of the polymer. Also, the contribution of interstitial and intracavity crystallization water molecules is reported. Solid-state NMR spectroscopy is used to study the molecular mobility of the polymer by measuring the 1H spin–lattice relaxation time in the rotating frame (T). The T values obtained for the polymer β-CDNS are compared with free β-CD. The observed relaxation parameters point out that the ester formation occurs mainly at the primary OH groups of CDs, also supporting the interpretation of vibrational spectra.

Keywords

Cyclodextrin nanospongesFTIR-ATR spectroscopyRaman spectroscopyO–H stretchingSolid state NMR spectroscopy

Copyright information

© Springer Science+Business Media B.V. 2012

Authors and Affiliations

  • F. Castiglione
    • 1
  • V. Crupi
    • 2
  • D. Majolino
    • 2
  • A. Mele
    • 1
    • 3
  • W. Panzeri
    • 4
  • B. Rossi
    • 5
  • F. Trotta
    • 6
  • V. Venuti
    • 2
  1. 1.Dipartimento di ChimicaMateriali e Ing. Chimica “G. Natta”, Politecnico di MilanoMilanoItaly
  2. 2.Dipartimento di FisicaUniversità di Messina, and CNISM, UdR MessinaMessinaItaly
  3. 3.CNR-Istituto di Chimica del Riconoscimento MolecolareMilanoItaly
  4. 4.CNR-Istituto di Chimica del Riconoscimento MolecolareMilanoItaly
  5. 5.Dipartimento di FisicaUniversità di TrentoPovo, TrentoItaly
  6. 6.Dipartimento di Chimica IFM Università di TorinoTorinoItaly