Cs. Triantafillidis et al., Effect of the degree and type of the dealumination method on the structural, compositional and acidic characteristics of H-ZSM-5 zeolites, MICROP M M, 47(2-3), 2001, pp. 369-388
A series of H-ZSM-5 zeolites with different framework Si/Al ratios were pre
pared by hydrothermal synthesis and post-synthesis dealumination by various
methods, i.e., HCl, steaming, steaming/HCl and ammonium hexafluorosilicate
(AHFS). The degree of framework dealumination and the amount/type of the e
xtra-framework phases formed were greatly dependent on the method of dealum
ination and the severity of the experimental conditions. The hydrothermal t
reatment of a parent ZSM-5 sample with Si/Al similar to 27 was very effecti
ve and produced significant amounts of Si-Al extra-framework phases, while
the reaction with HCl in relatively strongly acidic environments resulted i
n very low dealumination. Treatment with AHFS was proven to be an appropria
te method for preparing moderately dealuminated H-ZSM-5 samples which are f
ree from extra-framework Al. The relative crystallinity and the microporosi
ty of all dealuminated H-ZSM-5 zeolites were retained to a high degree (> 8
0%), even for the severely steamed samples (similar to 96% dealumination).
The morphology of the crystals/particles was not changed significantly; how
ever, each dealumination method had a different effect on the partial break
down of the crystals and on the formation of extra-framework/amorphous phas
es with a mesoporous character. The number of acid sites that corresponded
to the high-temperature desorption peak of the ammomia-temperature programm
ed desorption spectra was found to be equivalent to the framework Al (FA1)
content of all H-ZSM-5 samples, irrespective of the degree of dcalumination
and the amount of extra-framework phases. Theses phases had a low capabili
ty of adsorbing ammonia compared to the FA1 atoms and were the main source
of acidity for the severely steamed samples which had almost no FA1 (D 2001
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