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We introduce a nanoparticle assembly system for the preparation of homogeneous, ordered, mesoporous ZrO2–WO3 mixed oxides (denoted as mZW). Adding cationic surfactant Hexadecyl trimethyl ammonium Bromide (CTAB) process has been used to increase the Br(o)nsted acidic sites of mesoporous ZrO2–WO3 mixed oxides. mZW with 0.18 M CTAB as surfactant have as 5 times as much Br(o)nsted acidic sites as mZW without CTAB as surfactant, and exhibit significantly improved catalytic performance in Friedel–Crafts (F-C) reaction of anisole and benzyl alcohol which proceeds on strong or moderate strong Br(o)nsted acid sites. This originates from the Zr–WO3 cluster in ZrO2 crystal less than 10 nm induced by the addition of CTAB in mesoporous ZrO2–WO3 mixed oxides detected by STEM.