A hierarchical mesoporous ZSM-5 catalyst with aggregated nanocrystals structure was one-pot hydrothermally synthesized by using urea as the additive. The crystalline phase, morphology and hierarchical architectures were characterized by the XRD, SEM, TEM and N2 adsorption/desorption analyses. The nano-aggregates showed MFI crystalline phase and were composed of connected nanoparticles. The samples had the high surface area and the pore volume from intercrystalline among the nanoparticles due to spontaneously stacking of nanocrystals. The pyridine-adsorbed FTIR and the catalytic performances in the alkylation of phenol and tert-butyl alcohol were applied to evaluate the accessibility of acid sites and the catalytic activities for the hierarchical mesoporous ZSM-5 samples. The samples possessed high accessibility of acid sites which resulted from their large amount of mesopores, and its catalytic activity was improved dramatically. The phenol conversion could reach up to 95.6%, and the corresponding selectivity of 4-TBP and 2,4-DTBP was 44% and 51.5%, respectively.
