Aiming at the problems of time-consuming, low yield and low porosity of the original synthesis method of MIL-101, a new synthetic approach was proposed by using nitric acid as mineralizing agent via microwave irradiation method. The charatcterization and analysis results showed that the reaction time was shortened to 40 min (from original time of 8 h), and the product possessed ultra-high BET surface area of 3700 m2/g and excellent yield over 70% (compared with the original yield of 50%).