To alleviate environment issues derived from CO2 emission, developing effective and economical methods for CO2 capture has attracted much attention for decades. Metal-organic frameworks possess high porosity and stability, which is favorable to the adsorption of small molecules. Herein, an aluminumbased MOF, aluminum terephthalate [MIL-53(Al)], was synthesized with H2O and N,N0- dimethylformamide as co-solvent via microwave-assisted method for CO2 adsorption. The parameters including pre-mixing mode, microwave temperature, microwave power and reaction time were varied to study their influences on crystal structure, morphology and CO2 adsorption capacity of MW-MIL-53 (Al). Wherein, MW-MIL-53(Al) prepared with pre-mixing mode of stirring at 130 ℃, 200 W and 3 h presents high crystallinity and rod-like morphology. The synthesized MW-MIL-53(Al) possesses relatively high BET surface area (961 m2/g), pore volume (0.46 cm3/g) and thermal stability (up to 480 ℃), and its CO2 adsorption capacity is 2.16 mmol CO2/g adsorbent under 25 ℃ and 0.1 MPa, which is higher than CS-MIL-53(Al) synthesized via conventional solvothermal method at 130 ℃ for 48 h.