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Title: Investigation of Aluminum Site Changes of Dehydrated Zeolite H-Beta during a Rehydration Process by High Field Solid State NMR

Journal Article · · Journal of Physical Chemistry C, 119(3):1410−1417
DOI:https://doi.org/10.1021/jp509982r· OSTI ID:1184980

Aluminum site changes for dehydrated H-Beta zeolite during rehydration process are systematically investigated by ²⁷Al MAS and MQ MAS NMR at high magnetic fields up to 19.9 T. Benefiting from the high magnetic field, more detailed information is obtained from the considerably broadened and overlapped spectra of dehydrated H-beta zeolite. Dynamic changes of aluminum sites are demonstrated during rehydration process. In completely dehydrated H-Beta, invisible aluminum can reach 29%. The strength of quadrupole interactions for framework aluminum sites decreases gradually during water adsorption processes. The number of extra-framework aluminum (EFAL) species, i.e., penta- (34 ppm) and octa- (4 ppm) coordinated aluminum atoms rises initially with increasing water adsorption, and finally change into either tetra-coordinated framework or extra-framework aluminum in saturated water adsorption samples, with the remaining octa-coordinated aluminum lying at 0 and -4 ppm, respectively. Quantitative ²⁷Al MAS NMR analysis combined with ¹H MAS NMR indicates that some active EFAL species formed during calcination can reinsert into the framework during this hydration process. The assignment of aluminum at 0 ppm to EFAL cation and -4 ppm to framework aluminum is clarified for H-Beta zeolite.

Research Organization:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Environmental Molecular Sciences Lab. (EMSL)
Sponsoring Organization:
USDOE
DOE Contract Number:
AC05-76RL01830
OSTI ID:
1184980
Report Number(s):
PNNL-SA-105728; 47582; 47841; KC0302010
Journal Information:
Journal of Physical Chemistry C, 119(3):1410−1417, Journal Name: Journal of Physical Chemistry C, 119(3):1410−1417
Country of Publication:
United States
Language:
English

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