Article (Scientific journals)
Synthesis of star and H-shape polymers via a combination of cobalt-mediated radical polymerization and nitrone mediated radical coupling reactions
Detrembleur, Christophe; Debuigne, Antoine; Altintas, Ozcan et al.
2012In Polymer Chemistry, 3 (1), p. 135-147
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Keywords :
radical polymerization; cobalt-mediated radical polymerization (CMRP); nitroxide-mediated polymerization (NMP); star-shaped polymer
Abstract :
[en] Via consecutive cobalt-mediated radical polymerization (CMRP), nitrone-mediated radical coupling (NMRC) and copper catalyzed azide-alkyne cycloaddition (CuAAC), polymers with mikto-arm star and H-shape architecture were synthesized. Poly(vinyl acetate)40-block-poly(acrylonitrile)78-Co(acac)2 polymers were synthesized via CMRC and subsequently coupled using an alkyne functional nitrone. The coupling efficiency of the NMRC process was assessed employing N-tert-butyl a-phenyl nitrone (PBN), which is structurally very similar to the later employed coupling agent. Generally, coupling efficiencies of close to 90% or higher were observed in all cases. Since the coupling reaction yields triblock copolymers bearing an alkoxyamine functionality (and thus also an alkyne group) in the middle of the chain, well defined PEG conjugates could be obtained via CuAAC. Miktoarm star polymers of the structure (PVAc-b-PAN)2-PEG were generated as well as H-shaped material of the structure (PVAc-b-PAN)2-PEG-(PVAc-b-PAN)2 via conjugation with bifunctional PEG. In all cases, very narrow molecular weight material was obtained. Molecular weight analysis of the intermediate and the final products reveals that the hydrodynamic volume of the miktoarm star and the H-shaped materials is not substantially increased during the final conjugation reaction despite the fact that the absolute molecular weight increases by more than a factor of two in the latter case. Success of the conjugation reactions was confirmed via composition analysis via NMR.
Research center :
Center for Education and Research on Macromolecules (CERM)
Disciplines :
Chemistry
Materials science & engineering
Author, co-author :
Detrembleur, Christophe ;  Université de Liège - ULiège > Department of Chemistry > Center for Education and Research on Macromolecules (CERM)
Debuigne, Antoine  ;  Université de Liège - ULiège > Department of Chemistry > Center for Education and Research on Macromolecules (CERM)
Altintas, Ozcan;  Karlsruhe Institute of Technology (KIT), Germany > Preparative Macromolecular Chemistry
Conradi, Matthias;  University of Hasselt > Institute for Materials Research (IMO) > Polymer Reaction Design Group
Wong, Edgar H. H.;  Karlsruhe Institute of Technology (KIT), Germany > Preparative Macromolecular Chemistry
Jérôme, Christine  ;  Université de Liège - ULiège > Department of Chemistry > Center for Education and Research on Macromolecules (CERM)
Barner-Kowollik, Christopher;  Karlsruhe Institute of Technology (KIT), Germany > Preparative Macromolecular Chemistry
Junkers, Thomas;  University of Hasselt > Institute for Materials Research (IMO) > Polymer Reaction Design Group
Language :
English
Title :
Synthesis of star and H-shape polymers via a combination of cobalt-mediated radical polymerization and nitrone mediated radical coupling reactions
Publication date :
January 2012
Journal title :
Polymer Chemistry
ISSN :
1759-9954
eISSN :
1759-9962
Publisher :
Royal Society Chemistry, Cambridge, United Kingdom
Volume :
3
Issue :
1
Pages :
135-147
Peer reviewed :
Peer Reviewed verified by ORBi
Funders :
BELSPO - SPP Politique scientifique - Service Public Fédéral de Programmation Politique scientifique
F.R.S.-FNRS - Fonds de la Recherche Scientifique [BE]
FWO - Fonds Wetenschappelijk Onderzoek Vlaanderen [BE]
The Islamic Development Bank (IDB)
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