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Well-defined PDMAEA stars via Cu(0)-mediated reversible deactivation radical polymerisation
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Whitfield, Richard, Anastaskia, Athina, Truong, Nghia P., Wilson, Paul, Kempe, Kristian, Burns, James A., Davis, Thomas P. and Haddleton, David M. (2016) Well-defined PDMAEA stars via Cu(0)-mediated reversible deactivation radical polymerisation. Macromolecules, 49 (23). pp. 8914-8924. doi:10.1021/acs.macromol.6b01511 ISSN 0024-9297 .
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Official URL: http://doi.org/10.1021/acs.macromol.6b01511
Abstract
The Cu(0)-mediated reversible deactivation radical polymerisation of N,N’-dimethylaminoethyl acrylate in DMSO and IPA at ambient temperature using Cu(0) wire is investigated. Tetra-functional and octa-functional initiators were utilised to facilitate the synthesis of well-defined PDMAEA star homo and block copolymers with a range of molecular weights (Mn ~ 5000-41000 g mol-1). Both solvents demonstrated to be excellent media for the controlled polymerisation of DMAEA yielding narrow molecular weight distributions (Ð ~ 1.1) when the reactions were ceased at ~ 40% conversion. Interestingly, at high conversions (typically > 55%) high and low molecular weight shoulders were evident by SEC when DMSO and IPA were used respectively, suggesting large extent of termination and/or side reactions at prolonged reaction times. Nevertheless, high end group fidelity could be maintained when immediate precipitation of the polymers (at lower conversion) was performed yielding low dispersed P(DMAEA-b-MA) star block copolymers (Ð < 1.19, Mn ~ 20000 g mol-1). Importantly, guidelines on how to prevent hydrolysis, termination and side reactions of PDMAEA as well as how to purify and store such materials are also provided and discussed.
| Item Type: | Journal Article | ||||||||
|---|---|---|---|---|---|---|---|---|---|
| Subjects: | Q Science > QD Chemistry | ||||||||
| Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | ||||||||
| Library of Congress Subject Headings (LCSH): | Dimethylaminoethanol, Acrylates, Addition polymerization | ||||||||
| Journal or Publication Title: | Macromolecules | ||||||||
| Publisher: | American Chemical Society | ||||||||
| ISSN: | 0024-9297 | ||||||||
| Official Date: | 13 December 2016 | ||||||||
| Dates: |
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| Volume: | 49 | ||||||||
| Number: | 23 | ||||||||
| Page Range: | pp. 8914-8924 | ||||||||
| DOI: | 10.1021/acs.macromol.6b01511 | ||||||||
| Status: | Peer Reviewed | ||||||||
| Publication Status: | Published | ||||||||
| Access rights to Published version: | Restricted or Subscription Access | ||||||||
| Date of first compliant deposit: | 9 November 2016 | ||||||||
| Date of first compliant Open Access: | 15 November 2017 | ||||||||
| Funder: | University of Warwick, Australian Research Council (ARC), Syngenta UK (Firm), Advantage West Midlands (AWM), European Regional Development Fund (ERDF), Royal Society (Great Britain). Wolfson Research Merit Award (RSWRMA) | ||||||||
| Grant number: | Project number CE140100036 (ARC) |
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