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Synthesis of a well-defined polyelectrolyte by controlled/“living” nitroxide-mediated radical polymerization. Kinetic study

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Abstract The synthesis and characterization of potassium 4-styrenesulfonyl (trifluoromethylsulfonyl) imide (STFSIK) monomer as well as its controlled/living nitroxide-mediated radical polymerization (NMRP), using N-tert-Butyl-N-(2-methyl-1-phenylpropyl)-O-(1-phenylethyl) hydroxylamine as initiator in 50% w/v solutions… Click to show full abstract

Abstract The synthesis and characterization of potassium 4-styrenesulfonyl (trifluoromethylsulfonyl) imide (STFSIK) monomer as well as its controlled/living nitroxide-mediated radical polymerization (NMRP), using N-tert-Butyl-N-(2-methyl-1-phenylpropyl)-O-(1-phenylethyl) hydroxylamine as initiator in 50% w/v solutions of DMF at 125 °C, are reported. The kinetic studies of STFSIK indicated controlled/“living” polymerization process free of coupling and transfer reactions. 1H NMR and SEC were employed to determine the rate of monomer consumption and molecular weight distribution, Ð, of the synthesized samples. The polymerization reaction established high monomer conversion in just an hour with high end-group fidelity and the ability to continue polymerization with no visible terminations. Finally, the synthesis of the corresponding PSTFSILi homopolymer was achieved through a metathesis reaction between PSTFSIK and LiClO4, and the subsequent purification was successful against dialysis in water.

Keywords: polymerization; controlled living; radical polymerization; living nitroxide; nitroxide mediated; mediated radical

Journal Title: European Polymer Journal
Year Published: 2020

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