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

Polybetaines exhibit unique properties combining anti-polyelectrolyte and low protein fouling behaviour, as well as biocompatibility. To date, the synthesis of polybetaine particles >50 nm has proved to be extremely challenging with standard emulsion and dispersion techniques being unsuccessful....

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Main Authors: Bassett, Simon P., Birkin, Natasha A., Jennings, James, Champman, Emma, O'Reilly, Rachel K., Howdle, Steven M., Willcock, Helen
Format: Article
Published: Royal Society of Chemistry 2017
Online Access:https://eprints.nottingham.ac.uk/47250/
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author Bassett, Simon P.
Birkin, Natasha A.
Jennings, James
Champman, Emma
O'Reilly, Rachel K.
Howdle, Steven M.
Willcock, Helen
author_facet Bassett, Simon P.
Birkin, Natasha A.
Jennings, James
Champman, Emma
O'Reilly, Rachel K.
Howdle, Steven M.
Willcock, Helen
author_sort Bassett, Simon P.
building Nottingham Research Data Repository
collection Online Access
description Polybetaines exhibit unique properties combining anti-polyelectrolyte and low protein fouling behaviour, as well as biocompatibility. To date, the synthesis of polybetaine particles >50 nm has 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 3.0 × 10−2 mol L−1 and 1.8 × 10−1 mol L−1 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 was observed by SEM analysis for the optimised particles. The particles were readily re-dispersed in aqueous solution and light scattering measurements confirmed their low size dispersity.
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spelling nottingham-472502020-05-04T18:53:43Z https://eprints.nottingham.ac.uk/47250/ One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide Bassett, Simon P. Birkin, Natasha A. Jennings, James Champman, Emma O'Reilly, Rachel K. Howdle, Steven M. Willcock, Helen Polybetaines exhibit unique properties combining anti-polyelectrolyte and low protein fouling behaviour, as well as biocompatibility. To date, the synthesis of polybetaine particles >50 nm has 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 3.0 × 10−2 mol L−1 and 1.8 × 10−1 mol L−1 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 was observed by SEM analysis for the optimised particles. The particles were readily re-dispersed in aqueous solution and light scattering measurements confirmed their low size dispersity. Royal Society of Chemistry 2017-07-03 Article PeerReviewed Bassett, Simon P., Birkin, Natasha A., Jennings, James, Champman, Emma, O'Reilly, Rachel K., Howdle, Steven M. and Willcock, Helen (2017) One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide. Polymer Chemistry, 8 . pp. 4557-4564. ISSN 1759-9962 http://pubs.rsc.org/en/content/articlehtml/2017/py/c7py00455a doi:10.1039/C7PY00455A doi:10.1039/C7PY00455A
spellingShingle Bassett, Simon P.
Birkin, Natasha A.
Jennings, James
Champman, Emma
O'Reilly, Rachel K.
Howdle, Steven M.
Willcock, Helen
One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide
title One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide
title_full One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide
title_fullStr One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide
title_full_unstemmed One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide
title_short One-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide
title_sort one-pot synthesis of micron-sized polybetaine particles: innovative use of supercritical carbon dioxide
url https://eprints.nottingham.ac.uk/47250/
https://eprints.nottingham.ac.uk/47250/
https://eprints.nottingham.ac.uk/47250/