A series of Fe/MgO catalysts were prepared by impregnation method and characterized by XRD and CO2-TPD.Selective synthesis of acrylonitrile from acetonitrile and methanol was carried out in a conventional flow reactor system.The effects of Fe loading and reaction temperatures on the catalytic properties of Fe/MgO were studied.Experimental results show the catalytic properties was greatly improved by the addition of Fe to MgO.As Fe loading was 5%,it had the best catalytic property with conversion 22.6% of acetonitrile and with selectivity to acrylonitrile 81.9% at 400℃.Excess addition of Fe results in a decrease in activity and selectivity.CO2-TPD showed that stronger and less base sites on the surface of catalysts were both unfavorable for the reaction.