The synthesis of AB(2) Y-shaped amphiphilic block copolymers by macromolecular azo coupling reaction is reported. The hydrophobic block with the functional group at the end of the polymeric chain was prepared by controlled radical polymerization methods such as RAFT and ATRP. The hydrophilic block with diazonium salt group was obtained by the diazotization of V-shaped aniline-functionalized PEG. Then Y-shaped block copolymers were easily prepared through macromolecular azo coupling reactions between the abovementioned two polymeric blocks. The results of experiments showed that the position of the functional group suitable for azo coupling reaction in the polymeric chain has considerable effect on the efficiency of macromolecular azo coupling reaction. It was easier for the macromolecular diazonium salts to attack the functional groups when they were at the end of the macromolecular chains instead of in the middle. The self-assembly properties of the obtained Y-shaped amphiphilic block copolymers were also studied. Colloidal spheres were prepared by gradual hydrophobic aggregation of the polymeric chains in a THF-H2O dispersion medium.
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