The paper reports on the synthesis of a new bifunctional radicalic initiator and its behavior in the polymerization process. The synthesis of cumyl 4-t-butylazo-4-cyanoperoxypentanoate has been achieved by condensation of the corresponding acid chloride with cumen hydroperoxide. The structure of the azo perester is confirmed by IR, UV, and NMR spectra. The initiator has been used in styrene polymerization and the conversion of the polymer studied in connection to monomer and initiator concentration, time of reaction, and temperature. In compliance with multiple regression method, an equation correlating the PS conversion with the previously mentioned variables has been established.
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