Non-toxic nanomaterials have gained significant importance recently in the treatment of industrial wastewater that sometimes contains organic dyes such as methylene blue. We report here an easy approach for the synthesis of γ-alumina (Al₂O₃) nanoparticles via a method that incorporates the use of formamide and the non-ionic surfactant Tween-80. Together, formamide and Tween-80 serve as an effective precipitating agent and a convenient synthetic template, respectively, in directing the growth of the alumina nanoparticles. The morphology and structure of the nanoparticles were investigated by FT-IR, XRD, TGA, SEM, EDX, elemental mapping and TEM methods. The sizes of the nanoparticles are in the 30–50 nm range. The maximum pore size is 4.13 nm and the surface area is 112.9 m² g⁻¹ as determined by the Brunauer–Emmett–Teller (BET) method. The nanomaterials are excellent adsorbents for the cationic methylene blue dye from aqueous solution. The effects of pH, time, temperature and concentration on the adsorption have been examined and the adsorption capacity increased from 490 to 2210 mg g⁻¹ as the initial concentration was increased from 50 to 400 mg L⁻¹ under the following conditions: pH 9, 10 min reaction time, and 60 °C. The adsorption mechanism is considered to encompass electrostatic interactions in water between the Al₂O₃ nanoparticles and the cationic methylene blue dye. These readily made nanoparticles may well prove useful in both wastewater treatment and industrial catalysis.