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Journal of Porous Materials

, Volume 23, Issue 2, pp 339–348 | Cite as

Structural characterization of octadecyl modified MCM-41 silica by NMR and FTIR

  • Tahira Yasmin
  • Klaus Müller
Article
  • 252 Downloads

Abstract

Mesoporous MCM-41 silica spheres were prepared via the pseudomorphic route, using commercial prontosil silica spheres. Surface modification offers a great opportunity to adjust both the pore structure and surface properties of MCM-41 type materials which results in materials of improved hydrothermal and mechanical stability to make them promising candidates for chromatographic applications. In the present context, the obtained MCM-41 silica spheres were surface modified with octadecyl (C18) alkyl chains, by using direct grafting and surface polymerization methods, in order to vary the degree of surface hydrophobicity. The resulting materials were characterized before and after surface modification using various characterization techniques, with special emphasis on NMR and FTIR spectroscopies, for studying the attachment, mobility and the conformational order of the attached alkyl chains.

Keywords

MCM-41 Surface modification Spectroscopy 

Notes

Acknowledgments

The authors would like to thank Professor Dr. E. Roduner and Dr. A. Fels for the access to the BET and SEM instruments as well as Professor Dr. F. Gieβelmann for XRD measurements.

References

  1. 1.
    C.T. Kresge, M.E. Leonowicz, W.J. Roth, J.C. Vartuli, J.S. Beck, Nature 359, 710 (1992)CrossRefGoogle Scholar
  2. 2.
    J.S. Beck, J.C. Vartuli, W.J. Roth, M.E. Leonowicz, C.T. Kresge, K.D. Schmitt, C.T.-W. Chu, D.H. Olson, E.W. Sheppard, S.B. McCullen, J.B. Higgins, J.L. Schlenker, J. Am. Chem. Soc. 114, 10834 (1992)CrossRefGoogle Scholar
  3. 3.
    T. Martin, A. Galarneau, F. DiRenzo, F. Fajula, D. Plee, Angew. Chem. Int. Ed. 41, 2590 (2002)CrossRefGoogle Scholar
  4. 4.
    F. Fajula, A. Galarneau, F. Di Renzo, Microporous Mesoporous Mater. 82, 227 (2005)CrossRefGoogle Scholar
  5. 5.
    M. Grün, I. Lauer, K.K. Unger, Adv. Mater. 9, 254 (1997)CrossRefGoogle Scholar
  6. 6.
    I. Alonso-Lemus, Y. Verde-Gomez, A. Aguilar-Elguézabel, L. Alvarez-Contreras, J. Nanomater. 2010, 1 (2010)CrossRefGoogle Scholar
  7. 7.
    Z. Wang, J. Navarrete, Green Sustain. Chem. 2, 91 (2012)CrossRefGoogle Scholar
  8. 8.
    M.C. Bruzzoniti, C. Sarzanini, A.M. Torchia, M. Teodoro, F. Testa, A. Virga, B. Onida, J. Mater. Chem. 21, 369 (2011)CrossRefGoogle Scholar
  9. 9.
    H.B. Hassan, M.A. Rahim, M.W. Khalil, R.F. Mohammed, Int. J. Electrochem. Sci. 9, 760 (2014)Google Scholar
  10. 10.
    T. Martin, A. Galarneau, F. DiRenzo, D. Brunel, F. Fajula, S. Heinisch, G. Cretier, J.-L. Rocca, Chem. Mater. 16, 1725 (2004)CrossRefGoogle Scholar
  11. 11.
    C. Boissière, M. Kümmel, M. Persin, A. Larbot, E. Prouzet, Adv. Funct. Mater. 11, 129 (2001)CrossRefGoogle Scholar
  12. 12.
    A. Galarneau, J. Iapichella, D. Brunel, F. Fajula, Z. Bayram-Hahn, K.K. Unger, G. Puy, C. Demesmay, J.-L. Rocca, J. Sep. Sci. 29, 844 (2006)CrossRefGoogle Scholar
  13. 13.
    A. Kurganov, K.K. Unger, T. Issaeva, J. Chromatogr. A 753, 177 (1996)CrossRefGoogle Scholar
  14. 14.
    M. Raimondo, G. Perez, M. Sinibaldi, A. De Stefanis, A.A. Tomlinson, Chem. Commun. 15, 1343 (1997)CrossRefGoogle Scholar
  15. 15.
    C. Thoelen, K. Van de Walle, I.F.J. Vankelecom, P.A. Jacobs, Chem. Commun. 18, 1841 (1999)CrossRefGoogle Scholar
  16. 16.
    F. Fajula, Dalton Trans. 3, 291 (2007)CrossRefGoogle Scholar
  17. 17.
    N.I. Taib, S. Endud, M.N. Katun, Int. J. Chem. 3, 2 (2011)CrossRefGoogle Scholar
  18. 18.
    J.H. Clark, D.J. Macquarrie, Chem. Commun. 8, 853 (1998)CrossRefGoogle Scholar
  19. 19.
    X. Feng, G.E. Fryxell, L.-Q. Wang, A.Y. Kim, J. Liu, K.M. Kemner, Science 276, 923 (1997)CrossRefGoogle Scholar
  20. 20.
    M.H. Lim, C.F. Blanford, A. Stein, J. Am. Chem. Soc. 119, 4090 (1997)CrossRefGoogle Scholar
  21. 21.
    C.P. Jaroniec, M. Kruk, M. Jaroniec, A. Sayari, J. Phys. Chem. B 102, 5503 (1998)CrossRefGoogle Scholar
  22. 22.
    N. Linares, E. Serrano, M. Rico, A.M. Balu, E. Losada, R. Luque, J.M. Martı´nez, Chem. Commun. 47, 9024 (2011)CrossRefGoogle Scholar
  23. 23.
    A. Stein, B.J. Melde, R.C. Schroden, Adv. Mater. 12, 1403 (2000)CrossRefGoogle Scholar
  24. 24.
    Z.A. ALOthman, J. Mater. 5, 2874 (2012)CrossRefGoogle Scholar
  25. 25.
    R. Maoz, J. Sagiv, J. Colloid Interface Sci. 100, 465 (1984)CrossRefGoogle Scholar
  26. 26.
    S.R. Wasserman, G.M. Whitesides, I.M. Tidswell, B.M. Ocko, P.S. Pershan, J.D. Axe, J. Am. Chem. Soc. 111, 5852 (1989)CrossRefGoogle Scholar
  27. 27.
    U. Truedinger, G. Mueller, K.K. Unger, J. Chromatogr. 535, 111 (1990)CrossRefGoogle Scholar
  28. 28.
    M.J. Wirth, H.O. Fatunmbi, Anal. Chem. 65, 822 (1993)CrossRefGoogle Scholar
  29. 29.
    M. Pursch, L.C. Sander, K. Albert, Anal. Chem. 68, 4107 (1996)CrossRefGoogle Scholar
  30. 30.
    L.C. Sander, S.A. Wise, Anal. Chem. 56, 504 (1984)CrossRefGoogle Scholar
  31. 31.
    M. Pursch, R. Brindle, A. Ellwanger, L.C. Sander, C.M. Bell, H. Haendel, K. Albert, Solid State Nucl. Magn. Res. 9, 191 (1997)CrossRefGoogle Scholar
  32. 32.
    L.C. Sander, J.B. Kallis, L.R. Field, Anal. Chem. 55, 1068 (1983)CrossRefGoogle Scholar
  33. 33.
    S. Singh, J. Wegmann, K. Albert, K. Müller, J. Phys. Chem. B 106, 878 (2002)CrossRefGoogle Scholar
  34. 34.
    T. Yasmin, K. Müller, J. Chromatogr. A 1217, 3362 (2010)CrossRefGoogle Scholar
  35. 35.
    L. Jelinek, E.S. Kováts, Langmuir 10, 4225 (1994)CrossRefGoogle Scholar
  36. 36.
    L.Y. Zhang, F.L.Y. Lam, Z.F. Yan, X.J. Hu, Chin. J. Chem. Phys. 19, 102 (2006)CrossRefGoogle Scholar
  37. 37.
    L.C. Sander, S.A. Wise, Anal. Chem. 67, 3284 (1995)CrossRefGoogle Scholar
  38. 38.
    S. Zheng, L. Gao, J. Guo, Mater. Chem. Phys. 71, 174 (2001)CrossRefGoogle Scholar
  39. 39.
    Y.V. Subba Rao, D.E. De Vos, P.A. Jacobs, Angew. Chem. Int. Ed. Engl. 36, 2661 (1997)CrossRefGoogle Scholar
  40. 40.
    M. Grün, A.A. Kunganov, S. Schacht, F. Schüth, K.K. Unger, J. Chromatogr. A 740, 1 (1996)CrossRefGoogle Scholar
  41. 41.
    A. Galarneau, D. Desplantier, R. Dutartre, F. Di Renzo, Microporous Mesoporous Mater. 27, 297 (1999)CrossRefGoogle Scholar
  42. 42.
    A. Galarneau, J. Iapichella, K. Bonhomme, F. Di Renzo, P. Kooyman, O. Terasaki, F. Fajula, Adv. Funct. Mater. 16, 1657 (2006)CrossRefGoogle Scholar
  43. 43.
    J. Tudor, D. O’Hare, Chem. Commun. 6, 603 (1997)CrossRefGoogle Scholar
  44. 44.
    T.J. Barton, L.M. Bull, W.G. Klemperer, D.A. Loy, B. McEnaney, M. Misono, P.A. Monson, G. Pez, G.W. Scherer, J.C. Vartuli, O.M. Yaghi, Chem. Mater. 11, 2633 (1999)CrossRefGoogle Scholar
  45. 45.
    B.A. Grimes, S. Ludtke, K.K. Unger, A.I. Liapis, J. Chromatogr. A 979, 447 (2002)CrossRefGoogle Scholar
  46. 46.
    J. Iapichella, J.-M. Meneses, I. Beurroies, R. Denoyel, Z. Bayram-Hahn, K.K. Unger, A. Galarneau, Microporous Mesoporous Mater. 102, 111 (2007)CrossRefGoogle Scholar
  47. 47.
    Y. Ma, W. Tong, H. Zhou, L. Suib, Microporous Mesoporous Mater. 37, 243 (2000)CrossRefGoogle Scholar
  48. 48.
    K.T. Moller, C.D. Starr, S.A. Johnson, A Parent’s Guide to Cleft Lip and Palate (University of Minnesota Press, Minneapolis, 1990)Google Scholar
  49. 49.
    J.W. Wiench, Y.S. Avadhut, N. Maity, S. Bhaduri, G.K. Lahiri, M. Pruski, S. Ganapathy, J. Phys. Chem. B 111, 3877 (2007)CrossRefGoogle Scholar
  50. 50.
    M. Pursch, D.L. Vanderhart, L.C. Sander, X. Gu, T. Nguyen, S.A. Wise, D.A. Gajewski, J. Am. Chem. Soc. 122, 6997 (2000)CrossRefGoogle Scholar
  51. 51.
    G. Srinivasan, L.C. Sander, K. Müller, Anal. Bioanal. Chem. 384, 514 (2006)CrossRefGoogle Scholar
  52. 52.
    C.R. Kessel, S. Granick, Langmuir 7, 532 (1991)CrossRefGoogle Scholar
  53. 53.
    R.G. Snyder, M.W. Poore, Macromolecules 6, 708 (1973)CrossRefGoogle Scholar
  54. 54.
    A. Badia, L. Cuccia, L. Demers, F. Morin, R.B. Lennox, J. Am. Chem. Soc. 119, 2682 (1997)CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2015

Authors and Affiliations

  1. 1.Institut für Physikalische ChemieUniversität StuttgartStuttgartGermany
  2. 2.Dipartimento di Ingegneria dei Materiali e Tecnologie Industriali, INSTM, UdR TrentoUniversitá degli Studi di TrentoTrentoItaly

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