Microwave radiation process results in considerable energy savings compared with convectional heating methods. This study shows that styrene/acrylonitrile copolymerization reactions in solvent can be carried out rapidly using microwave radiation. It is new technology that strene/acrylonitrile was copolymerized by microwave energy with a change of microwave power, radiation time, monomer mole fraction etc. Conversion of styrene/acrylonitrile copolymer was shown from 3.91 to 40.92%. The maximum conversion was 40.92% at 130 W of microwave power, 120 min of reaction time and 0.006g of AIBN concentration.