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H Willcock Polymer Chemistry scCO2 2017.pdf (2.36 MB)

One-pot synthesis of micron-sized polybetaine particles; innovative use of supercritical carbon dioxide

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posted on 2017-07-27, 12:15 authored by Simon P. Bassett, Natasha A. Birkin, James Jennings, Emma Chapman, Rachel K. O'Reilly, Steven M. Howdle, Helen WillcockHelen Willcock
Polybetaines exhibit unique properties including anti-polyelectrolyte and low protein fouling behaviour, as well as biocompatibility. We recently presented the synthesis of ca. 20 nm polybetaine particles by aqueous RAFT polymerisation, but the synthesis of larger particles proved to be extremely challenging with standard emulsion and dispersion techniques being unsuccessful. Here we present the first reported synthesis of micron-sized, discrete cross-linked polybetaine particles, using polymerisation in scCO2 with methanol as a co-solvent. Discrete particles are produced only when the methanol is efficiently removed in-situ using scCO2 extraction. A relatively high crosslinking agent initial concentration (10 wt%) was found to result in the most well defined particles, and particle integrity reduced as the crosslinking agent initial concentration was decreased. A monomer loading of between 3.0x10-2 mol/L and 1.8x10-1 mol/L resulted in discrete micron sized particles, with significant agglomoration occuring as the monomer loading was increased further. A spherical morphology and extremely low size dispersity is observed by SEM analysis for the optimised particles. The particles are readily re-dispersed in aqueous solution and light scattering measurements confirm their low size dispersity.

History

School

  • Aeronautical, Automotive, Chemical and Materials Engineering

Department

  • Materials

Published in

Polymer Chemistry

Volume

8

Issue

31

Pages

4557 - 4564

Citation

BASSETT, S.P. ...et al., 2017. One-pot synthesis of micron-sized polybetaine particles; innovative use of supercritical carbon dioxide. Polymer Chemistry, 8 (31), pp. 4557-4564.

Publisher

© The Royal Society of Chemistry

Version

  • AM (Accepted Manuscript)

Publisher statement

This work is made available according to the conditions of the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) licence. Full details of this licence are available at: https://creativecommons.org/licenses/by-nc-nd/4.0/

Acceptance date

2017-07-02

Publication date

2017-07-03

Notes

This paper was published in the journal Polymer Chemistry and the definitive published version is available at http://dx.doi.org/10.1039/C7PY00455A.

ISSN

1759-9954

eISSN

1759-9962

Language

  • en

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