The intention of the work is develop novel polymeric materials by application of microreaction technology. A state-of-the-art pseudo anionic styrene polymerization was selected to test microreaction techniques. s-BuLi was used as initiator, cyclohexane as solvent and the reaction was carried out to 50 °C. The high heat and mass transfer allow a living polymerization without additives at high concentration and temperature. Thus the efficiency of the polymerization was increased significantly.