Zeolite beta crystals (Si/Al = 35) synthesized in fluoride medium were treated in aqueous 0.2 M NaOH solution for mesopore formation by selective extraction of framework silicon. A 16 parallel-batch reactor was used to study the influence of the treatment time and temperature on the physico-chemical properties of the zeolites, which were characterized by ICP-OES, XRD, N2 adsorption at 77 K, SEM, TEM, DRIFTS, and in situ ATR-IR. Alkaline treatment of H-beta within the optimal window of Si/Al ratios identified for other zeolite families leads to extensive silicon extraction at mild treatment conditions. This originates substantial mesoporosity and presumably improved transport, but negatively impacts on the microporous and acidic properties of the resulting sample. Consequently, the alkaline-treated beta zeolites show lower catalytic activity in the acid-catalyzed liquid-phase benzene alkylation than the purely microporous parent material. The relatively low stability of framework aluminum in BEA, compared to MFI and MOR, is detrimental for the controlled mesopore formation by Si dissolution, since aluminum cannot optimally exert its pore-directing role.
Mesoporous beta zeolite obtained by desilication
Micropor. Mesopor. Mat. 2008, 114, 93-102.