Distribution and mass transfer of phase transfer catalytic intermediate play an important role in phase transfer catalysis, Higher distribution ratio and fast mass transfer rate of active intermediate enhance the overall reaction rate in two-phase system. The behaviors of mass transfer and distribution of phase transfer catalytic intermediate in two-phase system were investigated in the present study. The effects of temperature, solvent, concentration of intermediate, and amounts of salts added on distribution were carried out in a batch vessel. The distribution constants increase with increasing initial concentration and temperature and were correlated as a function of equilibrium organic concentration. Overall mass transfer coefficients (K(QY)a) of catalytic intermediates from organic to aqueous phase for various agitating speeds and temperatures were obtained. A mathematical model concerning mass transfer in a single droplet was also developed to describe the dispersed phase system successfully.