A series of xAHFS/HMCM-22 (x denotes the amount of AHFS treatment on HMCM-22, AHFS is the abbreviation for ammonium hexafluorosilicate) were prepared and evaluated in the catalytic synthesis of p-cresol by alkylation of phenol with methanol. Several characterization techniques including N 2 adsorption-desorption, XRD, FT-IR, 27 Al MAS NMR, Pyridine-IR, and NH 3 -TPD have been used to analyze the physicochemical properties of the xAHFS/HMCM-22 catalyst. The conversion of phenol decreased with increasing x of xAHFS/HMCM-22 catalyst; while the selectivity for p-cresol maximized at x = 0.07. The 0.07AHFS/HMCM-22 catalyst was identified as the most efficient catalyst, showing the highest p-cresol selectivity (53.3 %) for longer than 24 h under optimized reaction conditions (325 °C, WHSV = 2 h À 1 ), which is much higher than that of parent HMCM-22 catalyst (37.1 %). The high p-cresol selectivity of the catalyst is attributed to AHFS removing part of the acid sites on the external surface of the HMCM-22, and preserving the acid sites in the micropores of zeolite. By contrast, the decrease in catalyst activity is due to the decrease in total acid sites.