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  Acid-Induced Room Temperature RAFT Polymerization: Synthesis and Mechanistic Insights

Vandenbergh, J., Schweitzer-Chaput, B., Klussmann, M., & Junkers, T. (2016). Acid-Induced Room Temperature RAFT Polymerization: Synthesis and Mechanistic Insights. Macromolecules, 49, 4124-4135. doi:10.1021/acs.macromol.6b00192.

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Vandenbergh, Joke1, Author
Schweitzer-Chaput, Bertrand2, Author              
Klussmann, Martin2, Author              
Junkers, Thomas1, 3, Author
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1Polymer Reaction Design Group, Institute for Materials Research (IMO), Hasselt University, Campus Diepenbeek, Building D, B-3590 Diepenbeek, Belgium, ou_persistent22              
2Research Group Klußmann, Max-Planck-Institut für Kohlenforschung, Max Planck Society, Max-Planck-Institut für Kohlenforschung, Kaiser-Wilhelm-Platz 1, 45470 Mülheim an der Ruhr, Germany, ou_persistent22              
3IMEC Division IMOMEC, Wetenschapspark 1, B-3590 Diepenbeek, Belgium, ou_persistent22              

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 Abstract: An acid-induced cyclohexanone/tert-butylhydroperoxide initiation system for ambient temperature reversible addition–fragmentation transfer (RAFT) polymerization of vinyl monomers is presented. The reaction system is optimized for the synthesis of poly(n-butyl acrylate) of various chain length. The polymerization shows typical living characteristics and polymers with dispersities close to 1.1 are obtained. Analysis of the polymer end groups by means of soft ionization mass spectrometry reveals the typical distribution of polymer containing both R and Z RAFT end groups and a minor distribution of a RAFT polymer carrying a cyclohexanone end group in α position. This observation demonstrates that the polymerization is initiated solely by ketone radicals despite a relatively complex initiation mechanism that involves several intermediates. The room temperature-derived homopolymers are successfully chain extended with tert-butyl acrylate resulting in well-defined block copolymer structures. To demonstrate the versatility of the approach, the room temperature RAFT polymerization is also applied to synthesize styrene and N-isopropylacrylamide, yielding best results for polystyrene. Finally, also a bisperoxide structure is tested as an alternative for the ketone/peroxide mixture. Polymerization proceeds substantially faster in this case and successful controlled polymerization to full conversion is achieved even at 0 °C. In general the proposed room temperature RAFT technique is very easy to carry out, in principle easily up scalable, metal free and shows high potential toward the synthesis of well-defined temperature sensitive materials.

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 Dates: 2016-05-202016
 Publication Status: Published in print
 Pages: 12
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 Table of Contents: -
 Rev. Type: Peer
 Identifiers: DOI: 10.1021/acs.macromol.6b00192
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Title: Macromolecules
Source Genre: Journal
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Publ. Info: Washington, D.C. : American Chemical Society
Pages: - Volume / Issue: 49 Sequence Number: - Start / End Page: 4124 - 4135 Identifier: ISSN: 0024-9297
CoNE: https://pure.mpg.de/cone/journals/resource/954925421108