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ZnCl2–aluminosilicate catalysts were prepared via a sol–gel route involving fluoride‐catalyzed hydrolysis of aluminum and silicon alkoxides in the presence of NaF, KF, NH4F and ZnF2. The catalysts were characterized by employing 29Si, 27Al and 19F solid‐state MAS NMR. The dependence of the activities of the catalysts on the nature and amount of fluoride present in the catalysts were investigated using Friedel–Crafts alkylation reaction of benzene with benzyl chloride.