Abstract
n-Butyl methacrylate has been polymerized in bulk at 130 °C in the presence of given amounts of a nitroxide stable free radical (TEMPO = 2,2,6,6-tetramethylpiperidine-N-oxyl) using either a low molar mass alkoxyamine initiator (2,2,6,6-tetramethyl-1-(1-phenethyloxy)piperidine) or a TEMPO-capped polystyrene macroinitiator. Complete consumption of both initiators was always observed. In contrast, very low final monomer conversions were found. Proton NMR spectroscopy and MALDI-TOF mass spectrometry were used for investigation of the polymer structure. They showed that the formed poly(n-butyl methacrylate) had the attached initiator at one end and that a block copolymer was synthesized when the polystyrene macroinitiator was used. The other terminal functionality of the polymer was not a TEMPO-based alkoxyamine but a methylene unsaturation exclusively. Particularly, no saturated polymer which would also be formed by conventional disproportionation reaction between two propagating radicals could be detected. F...
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