Advertisement

Thermal degradation of CTAB in as-synthesized MCM-41

  • J. Goworek
  • Agnieszka Kierys
  • W. Gac
  • Anna Borówka
  • R. Kusak
Article

Abstract

Thermal evacuation of a surfactant template from pure siliceous MCM-41 and MCM-41 containing aluminium in hydrogen flow was investigated. Micelle templated MCM-41 were prepared using hexadecyltrimethylammonium bromide (CTAB). The products of thermal surfactant degradation outside and inside pores were identified at various temperatures using 13C solid-state nuclear magnetic resonance (NMR) spectroscopy, gas chromatography coupled with mass spectrometer (GC-MS) and temperature programmed desorption coupled with mass spectrometer (TPD-MS). The GC-MS and 13C MAS NMR results obtained from this study provide an insight into the mechanism of surfactant transformation during MCM-41 synthesis on molecular level.

Keywords

CTAB GC-MS MAS NMR MCM-41 template removal 

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. 1.
    C. T. Kresge, M. E. Leonowicz, W. J. Roth, J. C. Vartuli and J. S. Beck, Nature, 359 (1992) 710.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 and J. L. Schlenker, J. Am. Chem. Soc., 114 (1992) 10834.CrossRefGoogle Scholar
  3. 3.
    S. A. Araujo, M. Ionashiro, V. J. Fernandes Jr. and A. S. Araujo, J. Therm. Anal. Cal., 64 (2001) 801.CrossRefGoogle Scholar
  4. 4.
    R. Denoyel, M. T. J. Keene, P. L. Llewellyn and J. Rouquerol, J. Therm. Anal. Cal., 56 (1999) 261.CrossRefGoogle Scholar
  5. 5.
    R. Zaleski, J. Wawryszczuk, A. Borówka, J. Goworek and T. Goworek, Micropor. Mesopor. Mater., 62 (2003) 47.CrossRefGoogle Scholar
  6. 6.
    M. J. B. Souza, A. O. S. Silva, J. M. F. B. Aquino, V. J. Fernandes Jr. and A. S. Araujo, J. Therm. Anal. Cal., 75 (2004) 693.CrossRefGoogle Scholar
  7. 7.
    T. Mori, Y. Kuroda, Y. Yoshikawa, M. Nagao and S. Kiitaka, Langmuir, 18 (2002) 1595.CrossRefGoogle Scholar
  8. 8.
    S. Ek, A. Root, M. Peussa and L. Niinisto, Thermochim. Acta, 379 (2001) 201.CrossRefGoogle Scholar
  9. 9.
    P. L. Llewellyn, Y. Grillet, J. Rouquerol, C. Martin and J.-P. Coulomb, Surf. Sci., 352-354 (1996) 468.CrossRefGoogle Scholar
  10. 10.
    M. J. Hudson and P. Trens, Characterization of Porous Solids V, Studies in Surface and Catalysis, K. K. Unger, et al., Eds, Vol. 128, The Royal Society of Chemistry, 2000, p. 505.Google Scholar
  11. 11.
    J. Ryczkowski, J. Goworek, W. Gac, S. Pasieczna and T. Borowiecki, Thermochim. Acta, 434 (2005) 2.CrossRefGoogle Scholar
  12. 12.
    F. Kleitz, W. Schmidt and F. Schüth, Micropor. Mesopor. Mater., 44–45 (2001) 95.CrossRefGoogle Scholar
  13. 13.
    F. Kleitz, W. Schmidt and F. Schüth, Micropor. Mesopor. Mater., 65 (2003) 1.CrossRefGoogle Scholar
  14. 14.
    M. T. Keene, R. D. M. Gougeon, R. Denoyel, R. K. Harris, J. Rouquerol and P. L. Llewellyn, J. Mater. Chem., 9 (1999) 2843.CrossRefGoogle Scholar
  15. 15.
    J. Wawryszczuk, J. Goworek, R. Zaleski and T. Goworek, Langmuir, 19 (2003) 2599.CrossRefGoogle Scholar
  16. 16.
    R. Zaleski, J. Wawryszczuk, J. Goworek, A. Borówka and T. Goworek, J. Colloid Interface Sci., 262 (2003) 466.CrossRefGoogle Scholar
  17. 17.
    R. Kumar, H.-T. Chen, J. L. V. Escoto, V. S.-Y. Lin and M. Pruski, Chem. Mater., 18 (2006) 4319.CrossRefGoogle Scholar
  18. 18.
    J. Goworek, A. Kierys and R. Kusak, Micropor. Mesopor. Mater., 98 (2007) 242.CrossRefGoogle Scholar
  19. 19.
    M. Grün, K. K. Unger, A. Matsumoto and K. Tsutsumi, B. McEnaney, J. T. Mays, J. Rouquerol, F. Rodriguez-Reinoso, K. S. W. Sing and K. K. Unger, Eds, Characterization of Porous Solids IV, The Royal Society of Chemistry, London 1997, p. 81.Google Scholar
  20. 20.
    M. M. L. Ribeiro Carrott, F. L. Conceição, J. M. Lopes, P. J. M. Carrott, C. Bernardes, J. Rocha and F. Ramôa Ribeiro, Micropor. Mesopor. Mater., 92 (2006) 270.CrossRefGoogle Scholar
  21. 21.
    E. P. Barrett, L. G. Joyner and P. P. Halenda, J. Am. Chem. Soc., 73 (1951) 373.CrossRefGoogle Scholar
  22. 22.
    M. Kruk, M. Jaroniec and A. Sayari, J. Phys. Chem. B, 101 (1997) 583.CrossRefGoogle Scholar
  23. 23.
    M. Kruk and M. Jaroniec, Chem. Mater., 13 (2001) 3169.CrossRefGoogle Scholar
  24. 24.
    J. Goworek, A. Deryło-Marczewska, W. Stefaniak, W. Zgrajka and R. Kusak, Mater. Chem. Phys., 77 (2002) 276.CrossRefGoogle Scholar
  25. 25.
    W. Lin, Q. Cai, W. Pang, Y. Yue and B. Zou, Micropor. Mesopor. Mater., 33 (1999) 187.CrossRefGoogle Scholar
  26. 26.
    A. Kierys, S. Pasieczna-Patkowska, J. Ryczkowski, A. Borówka and J. Goworek, The European Physical Journal — Special Topics, 154 (2008) 335.CrossRefGoogle Scholar
  27. 27.
    A. Jentys, K. Kleestorfer and H. Vinek, Micropor. Mesopor. Mater., 27 (1999) 321.CrossRefGoogle Scholar
  28. 28.
    M. J. B. Souza, A. O. S. Silva, V. J. Fernandes Jr. and A. S. Araujo, J. Therm. Anal. Cal., 79 (2005) 425.CrossRefGoogle Scholar
  29. 29.
    A. Araujo, V. Fernandes and S. Verissimo, J. Therm. Anal. Cal., 59 (2000) 649.CrossRefGoogle Scholar
  30. 30.
    M. Hunger, U. Schenk, M. Breuninger, R. Gläser and J. Weitkamp, Micropor. Mesopor. Mater., 27 (1999) 261.CrossRefGoogle Scholar
  31. 31.
    R. Ryoo, C. H. Ko and R. F. Howe, Chem. Mater., 9 (1997) 1607.CrossRefGoogle Scholar
  32. 32.
    Ch.-F. Cheng, W. Zhou and J. Klinowski, Chem. Phys. Lett., 263 (1996) 247.CrossRefGoogle Scholar
  33. 33.
    A. Sayari, Y. Yang, M. Kruk and M. Jaroniec, J. Phys. Chem. B, 103 (1999) 3651.CrossRefGoogle Scholar
  34. 34.
    A. Liepold, K. Roos, W. Reschetilowski, A. D. Esculcas, J. Roche, A. Philippow and A. W. Anderson, J. Chem. Soc. Faraday Trans., 92 (1996) 4623.CrossRefGoogle Scholar
  35. 35.
    A. Corma and A. Martinez, Handbook of Porous Solids, F. Schüth, K. S. W. Sing and J. Weitkamp, Eds, Wiley-VCH, Weinheim 2002, p. 2825.CrossRefGoogle Scholar
  36. 36.
    G. Leclercq, A. El Gharbi, L. Gengembre, T. Řomero, L. Leclercq and S. Pietrzyk, J. Catal., 148 (1994) 550.CrossRefGoogle Scholar
  37. 37.
    G. R. Bamwenda, Y. X. Zhao and B. W. Wojciechowski, J. Catal., 148 (1994) 595.CrossRefGoogle Scholar
  38. 38.
    L.-Q. Wang, J. Liu, G. J. Exarhos and B. C. Bunker, Langmuir, 12 (1996) 2663.CrossRefGoogle Scholar

Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2009

Authors and Affiliations

  • J. Goworek
    • 1
  • Agnieszka Kierys
    • 1
  • W. Gac
    • 2
  • Anna Borówka
    • 1
  • R. Kusak
    • 1
  1. 1.Department of Adsorption, Faculty of ChemistryMaria Curie-Skłodowska UniversityLublinPoland
  2. 2.Department of Chemical Technology, Faculty of ChemistryMaria Curie-Skłodowska UniversityLublinPoland

Personalised recommendations