Abstract Fundamental studies on the two-phase polycondensation using various phase-transfer catalysts such as quaternary ammonium and phosphonium salts, crown ethers, and poly(ethylene glycol)s yielded information useful for the synthesis of a variety of condensation polymers. We successfully synthesized various types of condensation polymers such as aromatic polysulfonates and polyphosphonates, aromatic polyethers, aliphatic and aromatic polysulfides, and carbon-carbon chain polymers of high molecular weights by the phase-transfer catalyzed polycondensation from combinations of aromatic disulfonyl chlorides, phosphonic di-chlorides, activated aromatic dichlorides, and aliphatic dihalides, with bisphenols, aliphatic and aromatic dithiols, and active methylene compounds. The two-phase polycondensation was generally carried out in a water-immiscible organic solvent-aqueous alkaline solution system at room temperature or above. In conclusion, this method of polycondensation offers a highly versatile and convenient synthetic method for a variety of condensation polymers.