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Journal of Porous Materials

, Volume 21, Issue 5, pp 659–665 | Cite as

Preparation and structural study of fully dehydrated, highly Mg2+-exchanged zeolite Y (FAU, Si/Al = 1.56) from undried methanol solution

  • Hu Sik Kim
  • Sang June Choi
  • Woo Taik Lim
Article
  • 168 Downloads

Abstract

Single-crystal of fully dehydrated, Mg2+-exchanged zeolite Y, |Mg34.5Na6|[Si117Al75O384]-FAU (Si/Al = 1.56), was successfully prepared from undried methanol solution (water concentration 0.02 M). A crystal of Na-Y was treated with 0.05 M MgCl2 ·6H2O in the solvent at 333 K, followed by vacuum dehydration at 723 K and 1 × 10−6 Torr for 2 days. Its structure was determined by single-crystal synchrotron X-ray diffraction techniques, in the cubic space group \(Fd\overline{3} m\) at 100 K. It was refined to the final error indices R 1/wR 2 = 0.0587/0.2210 with 1,294 reflections for which F o > 4σ(F o). In the structure of |Mg34.5Na6|[Si117Al75O384]-FAU, 34.5 Mg2+ ions per unit cell are found at four different crystallographic sites: 15 per unit cell are located at site I at the center of the hexagonal prism [Mg–O = 2.216(2) Å], two are at site I’ in the sodalite cavity near the hexagonal prism [Mg–O = 2.20(3) Å], only one is located at site II’ in the sodalite cavity [Mg–O = 2.197(23) Å], and the remaining 16.5 are at site II near single 6-oxygen rings in the supercage [Mg–O = 2.103(3) Å]. The residual 6 Na+ ions per unit cell are found at site II [Na–O = 2.218(7) Å]. No water molecules are found in this structure.

Keywords

Magnesium Zeolite Y Methanol Ion exchange Dehydrated 

Notes

Acknowledgments

The authors are grateful to the staff at beamline 2D SMC of the Pohang Light Source, Korea, for their assistance during data collection. This research was supported by the Basic Science Research Program through the National Research Foundation of Korea (NRF) as funded by the Ministry of Education, Science and Technology (Grant No. NRF-2012M2B2B1055496).

Supplementary material

10934_2014_9812_MOESM1_ESM.doc (1.3 mb)
Supplementary material 1 (DOC 1343 kb)

References

  1. 1.
    D. Break, Zeolite Molecular Sieves (Wiley, New York, 1974), p. 45Google Scholar
  2. 2.
    M. Sano, T. Maruo, H. Yamatera, M. Suzuki, Y. Saito, J. Am. Chem. Soc. 109, 52 (1987)CrossRefGoogle Scholar
  3. 3.
    S.B. Jang, Y. Kim, Bull. Korean Chem. Soc. 16, 539 (1995)Google Scholar
  4. 4.
    J. Warzywoda, M. Valcheva-Traykova, G.A. Rossetti Jr, N. Bac, R. Joesten, S.L. Suib, A. Sacco Jr, J. Cryst. Growth 220, 150 (2000)CrossRefGoogle Scholar
  5. 5.
    S.M. Seo, G.H. Kim, S.H. Lee, J.S. Bae, W.T. Lim, Bull. Korean Chem. Soc. 30, 1285 (2009)CrossRefGoogle Scholar
  6. 6.
    S.M. Seo, W.T. Lim, K. Seff, J. Phys. Chem. C 116, 13985 (2012)CrossRefGoogle Scholar
  7. 7.
    Y.F. Shepelev, A.A. Anderson, Y.I. Smolin, Zeolites 10, 61 (1990)CrossRefGoogle Scholar
  8. 8.
    Y.H. Yeom, S.B. Jang, Y. Kim, J. Phys. Chem. B 101, 6914 (1997)CrossRefGoogle Scholar
  9. 9.
    A.A. Anderson, Y.F. Shepelev, Y.I. Smolin, Zeolites 10, 32 (1990)CrossRefGoogle Scholar
  10. 10.
    H.S. Kim, S.O. Ko, W.T. Lim, Bull. Korean Chem. Soc. 32, 3696 (2011)CrossRefGoogle Scholar
  11. 11.
    Y. Kim, S.H. Lee, J.Y. Park, U.S. Kim, Bull. Korean Chem. Soc. 10, 349 (1989)Google Scholar
  12. 12.
    V. Crupi, D. Majolino, F. Longo, P. Migliardo, V. Venuti, Vib. Spectrosc. 42, 375 (2006)CrossRefGoogle Scholar
  13. 13.
    H.S. Kim, S.Y. Choi, W.T. Lim, J. Porous Mater. 20, 1449 (2013)CrossRefGoogle Scholar
  14. 14.
    W.T. Lim, S.M. Seo, L.Z. Wang, G.Q. Lu, N.H. Heo, K. Seff, Micropor. Mesopor. Mater. 129, 11 (2010)CrossRefGoogle Scholar
  15. 15.
    A.J. Arvai, C. Nielsen, ADSC Quantum-210 ADX Program (Area Detector System Corporation; Poway, CA, 1983)Google Scholar
  16. 16.
    Z. Otwinowski, W. Minor, Methods Enzymol. 276, 307 (1997)CrossRefGoogle Scholar
  17. 17.
    Bruker-AXS, (ver 6.12), XPREP, Program for the Automatic Space Group Determination, Bruker AXS Inc., Madison, WI, (2001)Google Scholar
  18. 18.
    G. M. Sheldrick, SHELXL97. Program for the Refinement of Crystal Structures (University of Gottingen, Germany, 1997)Google Scholar
  19. 19.
    W.T. Lim, S.Y. Choi, J.H. Choj, Y.H. Kim, N.H. Heo, K. Seff, Micropor. Mesopor. Mater. 92, 234 (2006)CrossRefGoogle Scholar
  20. 20.
    P.A. Doyle, P.S. Turner, Acta Crystallogr. Sect. A 24, 390 (1968)CrossRefGoogle Scholar
  21. 21.
    J.A. Ibers, W.C. Hamilton (eds.), International Tables for X-ray Crystallography, Vol. IV (Kynoch Press, Birmingham, 1974), pp. 71–98Google Scholar
  22. 22.
    D.T. Cromer, Acta Crystallogr. 18, 17 (1965)CrossRefGoogle Scholar
  23. 23.
    J. A. Ibers, W. C. Hamilton (eds.), International Tables for X-ray Crystallography, Vol. IV (Kynoch Press, Birmingham, 1974), pp. 148–150Google Scholar
  24. 24.
    W. Loewenstein, Am. Mineral. 39, 92 (1954)Google Scholar
  25. 25.
    D.W. Break, Zeolite Molecular Sieves (Wiley, New York, 1974), p. 93Google Scholar
  26. 26.
    H. Van Bekkum, E.M. Flanigen, P.A. Jacobs, J.C. Jansen, Introduction to Zeolites Science and Practice (Elsevier, 2001) p 44Google Scholar
  27. 27.
    Handbook of Chemistry and Physics, 70th edn., The Chemical Rubber Co.: Cleveland, OH, p. F-187 (1989/1990)Google Scholar
  28. 28.
    J. Plevert, F. Di Renzo, F. Fajula, J. Phys. Chem. B 101, 10340 (1997)CrossRefGoogle Scholar
  29. 29.
    M. Feuerstein, R.F. Lobo, Chem. Mater. 10, 2197 (1998)CrossRefGoogle Scholar
  30. 30.
    M. Feuerstein, R.J. Accardi, R.F. Lobo, J. Phys. Chem. B 104, 10281 (2000)CrossRefGoogle Scholar
  31. 31.
    H.S. Kim, D. Bae, W.T. Lim, K. Seff, J. Phys. Chem. C 116, 9009 (2012)CrossRefGoogle Scholar
  32. 32.
    H.S. Kim, S.O. Ko, W.T. Lim, Bull. Korean Chem. Soc. 33, 3303 (2012)CrossRefGoogle Scholar
  33. 33.
    H. Su, H.S. Kim, S.M. Seo, S.O. Ko, O.S. Lee, Y.H. Kim, W.T. Lim, Bull. Korean Chem. Soc. 33, 2785 (2012)CrossRefGoogle Scholar
  34. 34.
    Handbook of Chemistry and Physics, 77th edn., CRC Press Boca Raton, FL, p. 9–55 (1996/1997)Google Scholar
  35. 35.
    P.S. Albright, L.J. Gosting, J. Am. Chem. Soc. 68, 1061 (1946)CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2014

Authors and Affiliations

  1. 1.Department of Applied ChemistryAndong National UniversityAndongKorea
  2. 2.Department of Environmental EngineeringKyungpook National UniversityDaeguKorea

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