Solid-state NMR investigation of acid sites in dealuminated HZSM-5 zeolite
The acid sites and the hydration behaviors of dealuminated HZSM-5 zeolites (calcined at 550, 600, 650, and 700°C) were characterized by high-resolution 1H MAS, 1H{ 27A1} spin-echo double resonance in combination with 27A1 MAS NMR. Apart from the usually observed peaks for dealuminated zeolite HZSM-5...
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Published in | Magnetic resonance imaging Vol. 14; no. 7; pp. 945 - 946 |
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Main Authors | , , |
Format | Journal Article Conference Proceeding |
Language | English |
Published |
New York, NY
Elsevier Inc
1996
Elsevier Science |
Subjects | |
Online Access | Get full text |
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Summary: | The acid sites and the hydration behaviors of dealuminated HZSM-5 zeolites (calcined at 550, 600, 650, and 700°C) were characterized by high-resolution
1H MAS,
1H{
27A1} spin-echo double resonance in combination with
27A1 MAS NMR. Apart from the usually observed peaks for dealuminated zeolite HZSM-5, a narrow plus a broad peak simultaneously appears at ca.6.9 ppm in the
1H spectra and they exhibit different decay behavior in the
1H{
27A1} double-resonance experiments. The existence of the former signal indicates that Lewis acid sites may be formed in the zeolites after calcination. By means of the spin echo double resonance technique, we observed for the first time a previously unexpected narrow signal at 5.2 ppm, which resonates on the downfield side of Bronsted acid signal (4.3 ppm) and cannot be resolved in the
1H MAS spectra. This new signal is probably due to another kind of Bronsted acid site, locating in the small cages bounded by four- and five-membered rings. Three narrow peaks at 50 ppm, 30 ppm, and 0 ppm are superimposed on a very broad signal in the
27A1 MAS NMR spectra of dried HZSM-5. The intensity of the line at 50 ppm is significantly reduced compared with that of the rehydrated sample.
27A1 MAS NMR suggests that most part of the four-coordinated framework A1 turns into a intermediate case between four- and three-coordinated A1 after the dehydration and this process is reversible upon dehydration/rehydration. While some framework A1 atoms are transformed into three-coordinated A1 species and Lewis acid sites are, thus, generated in the dealuminated zeolites. For the signal at 30 ppm, the hydration leads to a dispersion in the chemical shift or the quadrupole interaction, which broadens its linewidth in hydrated samples. |
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Bibliography: | ObjectType-Article-1 SourceType-Scholarly Journals-1 ObjectType-Feature-2 content type line 23 |
ISSN: | 0730-725X 1873-5894 |
DOI: | 10.1016/S0730-725X(96)00189-0 |