Abstract
Synthesis of poly(ethylene adipate) (PEA) with 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) at both chain ends was attained by reaction of 4-hydroxy-TEMPO and PEA with isocyanate groups at the terminals. PEA obtained was found to have the living nitroxyl radical, because the electron spin resonance (ESR) spectrum of the polymer manifested a typical three sharp signals based on TEMPO. TEMPO-supported PEA served as a polymeric counter radical for the radical polymerization of styrene, to quantitatively give the block copolymer of ethylene adipate and styrene. Polymerization proceeded in accordance with a living mechanism, because the molecular weight of the copolymer was proportional to conversion of styrene and reciprocal of initial concentration of TEMPO attached to PEA. Analysis of the copolymer using a thin layer chromatography/flame ionization detection (TLC/FID) clarified that the copolymer contained no homopolystyrene. This absence of homopolystyrene implies that no diblock copolymer is formed during polymerization. 1H NMR analysis demonstrated the structure of copolymer obtained to be A-B-A triblock.
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