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Graft copolymers of hydroxyethyl cellulose by a ‘grafting to’ method :15N labelling as a powerful characterisation tool in ‘click’ polymer chemistry
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Joubert, Fanny, Musa, Osama, Hodgson, David R. W. and Cameron, Neil R. (2015) Graft copolymers of hydroxyethyl cellulose by a ‘grafting to’ method :15N labelling as a powerful characterisation tool in ‘click’ polymer chemistry. Polymer Chemistry, 6 (9). pp. 1567-1575. doi:10.1039/C4PY01413H ISSN 1759-9954.
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Official URL: http://dx.doi.org/10.1039/C4PY01413H
Abstract
We demonstrate how 15N labelling can be used to probe the success of ‘grafting to’ processes, through the preparation of well-defined graft copolymers of hydroxyethyl cellulose by combining RAFT polymerisation and copper-catalysed azide-alkyne cycloaddition (CuAAC). Using synthesised alkyne-functionalised chain transfer agents, short-chain (DP = 10) poly(N-vinylpyrrolidone) (PVP) and poly(N-isopropyl acrylamide) (PNIPAAM) were prepared in high conversion in a controlled manner (ĐM of ∼1.4 and 1.2 respectively). Separately, partially 15N-labelled N3-HEC was synthesised and characterised using solid state 13C, 15N CP-MAS NMR and FTIR spectroscopies. Alkyne-terminated PVP and PNIPAAM were grafted at different graft densities onto partially 15N-labelled N3-HEC using the click reaction. The hybrid HEC-g-polymer materials were fully characterised using solid state 13C and 15N CP-MAS NMR and FTIR spectroscopies. While 13C and FTIR spectroscopies gave indirect or weak evidence of CuAAC coupling, the cycloaddition of the alkyne-terminated polymers with N3-HEC was proven unambiguously by 15N solid state NMR spectroscopy. This indicates the utility of 15N labelling for probing the coupling efficiency of CuAAC reactions when employed in ‘grafting to’ processes with cellulosic substrates.
Item Type: | Journal Article | ||||||||||
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Subjects: | Q Science > QD Chemistry | ||||||||||
Divisions: | Faculty of Science, Engineering and Medicine > Engineering > Engineering | ||||||||||
Library of Congress Subject Headings (LCSH): | Graft copolymers, Polymers, Cellulose , Polymerization, Nuclear magnetic resonance spectroscopy | ||||||||||
Journal or Publication Title: | Polymer Chemistry | ||||||||||
Publisher: | Royal Society of Chemistry | ||||||||||
ISSN: | 1759-9954 | ||||||||||
Official Date: | 7 March 2015 | ||||||||||
Dates: |
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Volume: | 6 | ||||||||||
Number: | 9 | ||||||||||
Page Range: | pp. 1567-1575 | ||||||||||
DOI: | 10.1039/C4PY01413H | ||||||||||
Status: | Peer Reviewed | ||||||||||
Publication Status: | Published | ||||||||||
Access rights to Published version: | Restricted or Subscription Access | ||||||||||
Date of first compliant deposit: | 19 January 2017 | ||||||||||
Date of first compliant Open Access: | 19 January 2017 | ||||||||||
Funder: | Engineering and Physical Sciences Research Council (EPSRC), Ashland (Firm) |
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