Nanofiber-like mesoporous ?-Al2O3 was synthesized using freshly prepared boehmite sol in the presence of triblock copolymer, P123 following evaporation-induced self-assembly (EISA) process followed by calcinations at 400 degrees C1000 degrees C. The samples were characterized by thermogravimetry (TG), differential thermal analysis (DTA), X-ray diffraction (XRD), N2 adsorptiondesorption, and transmission electron microscopy (TEM). The adsorption efficiency of the samples with Congo red (CR) was studied by UVvis spectroscopy. XRD results showed boehmite phase in the as-prepared sample while ?-Al2O3 phase obtained at 400 degrees C was stable up to 900 degrees C, a little transformation of ?-Al2O3 resulted at 1000 degrees C. The Brunauer-Emmett-Teller surface area of the 400 degrees C-treated sample was found to be 175.5 m2g-1. The TEM micrograph showed nanofiber-like morphology of ?-Al2O3. The 400 degrees C-treated sample showed about 100% CR adsorption within 60 min.