A non-aqueous suspension polycondensation method was proposed to proceed the reaction of p -phenylenediamine and terephthaloyl chloride for the preparation of poly( p -phenylene terephthalamide) (PPTA). The system was operated with NMP-CaCl 2 solution as the dispersed phase and inert liquid paraffin as the continuous phase. Each of NMP-CaCl 2 solution microdroplet suspended in paraffin served as a microreactor where the polycondensation took place. According to the results of TGA, XRD, IR, SEM and EA, PPTA with good quality was obtained through this novel method, and a number of main factors influencing this process were investigated to determine the optimum condition for the preparation of PPTA. Besides, this two-phase polycondensation system brings many unique advantages compared to the conventional solution polycondensation method, including a sealed reaction environment keeping the reactants away from oxygen and water, easy removal of HCl to promote the reaction, well-controlled temperature and low viscosity which means less energy cost.