Gas-phase synthesis and characterization of CH4-loaded hydroquinone clathrates

Jong Won Lee, Yongjae Lee, Satoshi Takeya, Taro Kawamura, Yoshitaka Yamamoto, Yun Je Lee, Ji Ho Yoon

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27 Citations (Scopus)

Abstract

A CH4-loaded hydroquinone (HQ) clathrate was synthesized via a gas-phase reaction using the a-form of crystalline HQ and CH4 gas at 12 MPa and room temperature. Solid-state 13C cross-polarization/magic angle spinning (CP/MAS) NMR and Raman spectroscopic measurements confirm the incorporation of CH4 molecules into the cages of the HQ clathrate framework. The chemical analysis indicates that about 69% of the cages are filled by CH4 molecules, that is, 0.69 CH4 per three HQ molecules. Rietveld refinement using synchrotron X-ray powder diffraction (XRD) data shows that the CH4-loaded HQ clathrate adopts the /3-form of HQ clathrate in a hexagonal space group R3 with lattice paramet ers of a = 16.6191 Å and c = 5.5038 Å. Timeresolved synchrotron XRD and quadrupole mass spectroscopic measurements show that the CH4-loaded HQ clathrate is stable up to 368 K and gradually transforms to the a-form by releasing the confined CH4 gases between 368-378 K. Using solid-state 13C CP/MAS NMR, the reaction kinetics between the a-form HQ and CH4 gas is qualitatively described in terms of the particle size of the crystalline HQ,

Original languageEnglish
Pages (from-to)3254-3258
Number of pages5
JournalJournal of Physical Chemistry B
Volume114
Issue number9
DOIs
Publication statusPublished - 2010 Mar 11

All Science Journal Classification (ASJC) codes

  • Physical and Theoretical Chemistry
  • Surfaces, Coatings and Films
  • Materials Chemistry

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    Lee, J. W., Lee, Y., Takeya, S., Kawamura, T., Yamamoto, Y., Lee, Y. J., & Yoon, J. H. (2010). Gas-phase synthesis and characterization of CH4-loaded hydroquinone clathrates. Journal of Physical Chemistry B, 114(9), 3254-3258. https://doi.org/10.1021/jp911822e