Abstract: Ni/Al₂O₃ catalyst with various NiO loading was prepared with impregnation method. The catalytic performance for hydrogenation of 2-methylfuran to 2-methyltetrahydrofuran was investigated in this work. The results indicated that with an increase of NiO contents (10%, 20%, 25%, 30% and 40%), 2-methylfuran conversion rate first increased and then droped to a low level. The selectivity of this hydrogenation reaction showed the same trend. It was mainly because that NiO can produce more active center on catalyst surface, which was good for hydrogenation reaction. However, overloading of NiO blocked the mesopores of supportive Al₂O₃, and thus reduce the reaction selectivity and conversion rate. In batch reactor, after optimization the hydrogenation selectivity rate can be improved under hydrogen partial pressure of 3 MPa, reaction temperature of 150℃ and stirring speed of 1000 r/min. As a result, 2-methyltetrahydrofuran selectivity of 97.1% and 2-methylfuran conversion rate of 99.4% can be achieved with 25% NiO loading.