A facile route is initiated to fabricate well-defined mesoporous γ-Al 2 O 3 , with a three-dimensional micro/nanostructure, using basic aluminum sulfate (BAS) microcubes as precursor. The as-synthesized γ-Al 2 O 3 is cubic-like in morphology with an average size of ca. 6μm. Mesoporous γ-Al 2 O 3 synthesized by this method is highly thermal stable and exhibits superior adsorption performance (maximum adsorption capacity 9.93mg/g) with good recycling efficiency (more than 76% of its original adsorption capacity after 4 cycles) as an adsorbent to remove the heavy metal ions Cr(VI) as a result of its unique structure, which made it to be a promising material for environmental remediation.