Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
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MAS NMR and XRD Study on the Vanadium Site pf Vanadium Silicate Mesoporous Molecular Sieve MCM-41

  • Published : 1997.01.20
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Abstract

A wide range (10 < Si/V) of mesoporous vanadium silicate molecular sieves with the MCM-41 structure have been synthesized using vanadyl sulfate as the source of vanadium and characterized by XRD, 51V MAS NMR and 29Si MAS NMR. The increase of the unit cell parameter and the decrease of Q3/Q4 ratio of 29Si spectra with the vanadium content suggest the incorporation of vanadium in the framework of MCM-41 structure. 51V MAS NMR demonstrates that vanadiums in as-synthesized V-MCM-41 are present in the chemical environment of octahedra and octahedral vanadium is decreased and tetrahedral vanadium is increased inversely with raising the calcination temperature. Though the thermal treatment in rotor of hydrated sample resulted in the change from tetrahedral environment to octahedral one and the steaming and the acid treatment affect to the chemical environment of vanadium, the spectrum similar to originally calcined sample is regenerated after recalcination. This indicates that the vanadium is belong to the framework in a relatively exposed site. The best quality XRD pattern of the product of Si/V=27 may be attributable to heterogeneous nucleation mechanism. V-MCM-41's having the Si/V ratio lower than 20 are completely collapsed after calcination.

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References

  1. Nature v.359 Kresge, C. T.;Leonowicz, M. E.;Roth, W. J.;Vartuli, J. C.;Beck, J. S.
  2. J. Am. Chem. Soc. v.114 Beck, J. S.;Vartuli, J. C.;Roth, W. J.;Leonowicz, M. E.;Kresge, C. T.;Schmitt, K. D.;Chu, C. T.-W.;Olson, D. H.;Sheppard, E. W.;McCullen, S. B.;Higgins, J. B.;Schlenker, J. L.
  3. J. Chem. Soc., Chem. Commun. Corma, A.;Navarro, M. T.;Perez-Pariente, J.
  4. Surf. Sci. Catal. v.84 Franke, O.;Rathousky, J.;Schulz-Ekloff, G.;Starek, J.;Zukal, A. Stud
  5. J. Chem. Soc., Chem. Commun. Reddy, K. M.;Moudrakovski, I.;Sayari, A.
  6. J. Chem. Soc., Chem. Commun. Reddy, J. S.;Sayari, A.
  7. J. Phys. Chem. v.100 Cheng, C.-F.;He, H.;Zhou, W.;Klinowski, J.;Goncalves, J. A. S.;Gladden, L. F.
  8. J. Chem. Soc., Chem. Commun. Zhao, D. Y.;Goldfarb, D.
  9. Chem. Mater. v.7 Sayari, A.;Danuman, C.;Moudrakovski, I. L.
  10. J. Chem. Soc., Chem. Commun. Yuan, J. Y.;Liu, S. Q.;Chen, T. H.;Wang, J. Z.;Li, H. X.
  11. Stud. Surf. Sci. Catal. v.49 Miyamoto, A.;Iwamoto, Y.;Matsuda, H.;Inui, T.
  12. Zeolites v.8 Cavani, F.;Trifiro, F.;Habersberger, K.;Tvaruzkova, Z.
  13. Appl. Catal. v.19 Tvaruzcova, Z.;Centi, G.;Jiru, P.;Trifiro, F.
  14. Stud. Surf. Sci. Catal. v.49 Zatorski, L. W.;Centi, G.;Neito, J. L.;Trifiro, F.;Bellussi, G.;Fattore, V.
  15. Microporous Mater. v.2 Chen, C.-Y.;Li, H.-X.;Davis, M. E.
  16. J. Phys. Chem. v.97 Whittington, B. I.;Anderson, J. R.
  17. J. Catal. v.143 Reddy, K. R.;Ramaswamy, A. V.;Ratnasamy, P.
  18. J. Phys. Chem. v.96 Centi, G.;Perathoner, S.;Trifiro, F.;Aboukais, A.;Aissi, C. F.;Guelton, M.
  19. J. Catal. v.141 Prasada Rao, P. R. H.;Ramaswamy, A. V.;Ratnasamy, P.
  20. Appl. Catal. A.: General v.102 Tuel, A.;Ben Tarrit, Y.
  21. J. Catal. v.137 Hari Prasad Rao, P. R.;Ramaswamy, A. V.;Ratnasamy, P.
  22. J. Phys. Chem. v.99 Luan, Z.;Cheng, C.-F.;Zhou, W.;Klinowski, J.
  23. Zeolites, Synthesis, Structure, Technology and Application Barrer, R. M.;Drzaj, B.(ed.);Hocevar, S.(ed.);Pejovnik, S.(ed.)
  24. Recent Advances in Zeolite Science Kessler, H.;Klinowksi, J.(ed.);Barrie, P. J.(ed.)
  25. Langmuir v.11 Liu, J.;Kim, A. Y.;Virden, J. W.;Bunker, C.
  26. High Resolution Solid-State NMR of Silicates and Zeolites Engelhard, G.;Michel, D.
  27. Progr. NMR Spectrosc. v.24 Lapina, O. B.;Mastikhin, V. M.;Shubin, A. A.;Krasilnikov, V. N.;Zamarav, K.
  28. Appl. Catal. v.68 Rigutto, M. S.;van Bekkum, H.
  29. Kinet. Katal. v.11 Mastikhin, V. M.;Polyakova, G. M.;Ziolkowsky, J.;Borescov, G. K.
  30. Catal. Lett. v.13 Lapina, O. B.;Mastikhin, V. M.;Nosov, A. V.;Beutel, T.;Knozinger, H.
  31. J. Phys. Chem. v.92 Taouk, B.;Guelton, M.;Grimblot, J.;Bonnelle, J. P.
  32. J. Phys. Chem. v.93 Eckert, H.;Wachs, I. E.
  33. J. Phys. Chem. v.97 Das, N. D.;Eckert, H.;Hu, H.;Wachs, I. E.;Walzer, J. F.;Feber, F. J.
  34. Angew. Chem. Int. Ed. Engl. v.34 Chen, J.;Li, Q.;Xu, R.;Xiao, F.