Three types of Fe 2 O 3 /MgO (FeMgO IM , FeMgO Co and FeMgO HY ) nanomaterials were prepared by impregnation, co-precipitation and hydrothermal methods, respectively. The microporous FeMgO adsorbents were successfully used to remove synthetic textile dye (Remazol Red RB-133) by adsorption from aqueous solution. The as-prepared adsorbents were characterized by XRD, FT-IR, N 2 adsorption/desorption isotherms and TEM techniques. The results showed that a nanorod-like shape with high surface area and porous structure was obtained by hydrothermal treatment. The Langmuir and Freundlich adsorption models were applied to describe the equilibrium isotherms. The equilibrium adsorption data were best fitted by Langmuir isothermal model. The removal efficiencies of dye of 50mgL −1 within 19min can be ranked as: FeMgO HY >FeMgO IM >FeMgO Co . Also, the results indicated that pseudo-first-order and intra-particle diffusion models can better describe the adsorption kinetics. The microporous FeMgO HY and FeMgO IM were found to be effective adsorbent for the removal of dye from aqueous solution due to their increase in the microporosity as well as modified surface morphologies. The highly active FeMgO HY nanomaterial was evaluated for chemical oxygen demand (COD) and color reduction of a real industrial wastewater. A reduction in color and COD of 87% and 40%, respectively was achieved after 3h from adsorption.