Reactivity of extra-framework species of USY zeolites in alkaline medium

Research output: Contribution to journalArticleResearchpeer review

Authors

  • Wolfgang Lutz
  • Rainer Bertram
  • Detlef Heidemann
  • Rolf Kurzhals
  • Claus Rüscher
  • Galina Kryukova

Research Organisations

External Research Organisations

  • Brandenburg University of Technology
  • Leibniz Institute for Crystal Growth (IKZ)
  • Humboldt-Universität zu Berlin (HU Berlin)
  • Clariant AG
  • Boreskov Institute of Catalysis SB RAS
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Details

Original languageEnglish
Pages (from-to)75-82
Number of pages8
JournalZeitschrift fur Anorganische und Allgemeine Chemie
Volume637
Issue number1
Early online date8 Sept 2010
Publication statusPublished - Jan 2011

Abstract

Zeolites of type USY (ultra-stable Y) were obtained by steaming of NH 4NaY modification. Samples were modified by subsequent alkaline treatment in KOH solution. USY and USY-KOH were characterised by chemical element analysis, XRD, IR, 29Al and 29Si MAS NMR spectroscopic measurements. Correct silicon to aluminium ratios (Si/Al) were determined by XRD and IR (double ring vibration wDR) data whereas values calculated according to data of 29Si MAS NMR and IR spectroscopy (asymmetrical TOT valence vibration wTOT) appeared to be too high., In the latter case, the signals of the zeolite framework were strongly superimposed by that of extra-framework silica gel (EFSi) formed during steaming. It was found that alkaline leaching induces desilication of silicon-rich area of the zeolite framework and partial dissolution of EFSi. Silicate ions of both react with likewise dissolved extra-framework aluminium (EFAl) to form X-ray amorphous aluminosilicate. Consequently, the superposition of the 29Si MAS NMR signals of the zeolite framework by silica gel was reduced for Q4(0Al) but increased for Q4 (2Al) and Q4(3Al) structure units. A reinsertion of EFAl into the zeolite framework has not been observed.

Keywords

    Aluminum, Alumosilicates, NMR spectroscopy, Silicon, Synthesis design, Zeolites

ASJC Scopus subject areas

Cite this

Reactivity of extra-framework species of USY zeolites in alkaline medium. / Lutz, Wolfgang; Bertram, Rainer; Heidemann, Detlef et al.
In: Zeitschrift fur Anorganische und Allgemeine Chemie, Vol. 637, No. 1, 01.2011, p. 75-82.

Research output: Contribution to journalArticleResearchpeer review

Lutz, W, Bertram, R, Heidemann, D, Kurzhals, R, Rüscher, C & Kryukova, G 2011, 'Reactivity of extra-framework species of USY zeolites in alkaline medium', Zeitschrift fur Anorganische und Allgemeine Chemie, vol. 637, no. 1, pp. 75-82. https://doi.org/10.1002/zaac.201000273
Lutz, W., Bertram, R., Heidemann, D., Kurzhals, R., Rüscher, C., & Kryukova, G. (2011). Reactivity of extra-framework species of USY zeolites in alkaline medium. Zeitschrift fur Anorganische und Allgemeine Chemie, 637(1), 75-82. https://doi.org/10.1002/zaac.201000273
Lutz W, Bertram R, Heidemann D, Kurzhals R, Rüscher C, Kryukova G. Reactivity of extra-framework species of USY zeolites in alkaline medium. Zeitschrift fur Anorganische und Allgemeine Chemie. 2011 Jan;637(1):75-82. Epub 2010 Sept 8. doi: 10.1002/zaac.201000273
Lutz, Wolfgang ; Bertram, Rainer ; Heidemann, Detlef et al. / Reactivity of extra-framework species of USY zeolites in alkaline medium. In: Zeitschrift fur Anorganische und Allgemeine Chemie. 2011 ; Vol. 637, No. 1. pp. 75-82.
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abstract = "Zeolites of type USY (ultra-stable Y) were obtained by steaming of NH 4NaY modification. Samples were modified by subsequent alkaline treatment in KOH solution. USY and USY-KOH were characterised by chemical element analysis, XRD, IR, 29Al and 29Si MAS NMR spectroscopic measurements. Correct silicon to aluminium ratios (Si/Al) were determined by XRD and IR (double ring vibration wDR) data whereas values calculated according to data of 29Si MAS NMR and IR spectroscopy (asymmetrical TOT valence vibration wTOT) appeared to be too high., In the latter case, the signals of the zeolite framework were strongly superimposed by that of extra-framework silica gel (EFSi) formed during steaming. It was found that alkaline leaching induces desilication of silicon-rich area of the zeolite framework and partial dissolution of EFSi. Silicate ions of both react with likewise dissolved extra-framework aluminium (EFAl) to form X-ray amorphous aluminosilicate. Consequently, the superposition of the 29Si MAS NMR signals of the zeolite framework by silica gel was reduced for Q4(0Al) but increased for Q4 (2Al) and Q4(3Al) structure units. A reinsertion of EFAl into the zeolite framework has not been observed.",
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AU - Lutz, Wolfgang

AU - Bertram, Rainer

AU - Heidemann, Detlef

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AU - Rüscher, Claus

AU - Kryukova, Galina

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