Macroazoinitiator (MAI) was prepared from hydroxy-terminated polybutadiene (HTPB) and 4,4 ' -azobis-4-cyanopentanoic acid (ACPA) by direct polycondensation in the presence of 1-methyl-2-chloropyridinium iodide (MCPI) at room temperature. This MM proved to be an effective initiator for thermal polymerization of styrene at 60 degreesC. The resulting products were characterized by viscosity measurements and both IR and NMR spectral studies. The ratio of styrene and butadiene units was calculated from NMR spectral data and scanning electron micrography.