Free radical interfacial copolymerization which is carried out by means of an amphiphilic bifunctional initiator as a novel polymerization method was proposed for the first time. For utilizing the new polymerization method, an amphiphilic bifunctional initiator, palmitoyl (3-carboxy propionyl) sebacoyl diperoxide (PSD), was synthesized and further used to initiate the free radical interfacial copolymerization of acrylamide (AM) with n-butyl methacrylate (n-BMA) which gave the amphiphilic PAM/PnBMA block copolymers. The resulting PAM/PnBMA block copolymers were purified by solvent extraction and characterized by elemental analysis, solubility, IR and DSC.