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Current-controlled ‘plug-and-play’ electrochemical atom transfer radical polymerization of acrylamides in water
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Mohammed, Mahir, Jones, Bryn and Wilson, Paul (2022) Current-controlled ‘plug-and-play’ electrochemical atom transfer radical polymerization of acrylamides in water. Polymer Chemistry, 13 (23). pp. 3460-3470. doi:10.1039/D2PY00412G ISSN 1759-9954.
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WRAP-current-controlled-‘plug-and-play’-electrochemical-atom-transfer-radical-polymerization-acrylamides-water-Wilson-2022.pdf - Published Version - Requires a PDF viewer. Available under License Creative Commons Attribution. Download (765Kb) | Preview |
Official URL: http://dx.doi.org/10.1039/D2PY00412G
Abstract
Aqueous electrochemical atom transfer radical polymerisation (eATRP) can be challenging due to deleterious side reactions leading to the loss of the ω-chain end, increased rates of activation (k¬act) leading to higher [Pn˙] and increased rates of termination and lability of the X-CuII/L bond to hydrolysis leading to poor control. Here, we build on recent advances in eATRP methodology to develop a simplified current controlled eATRP of acrylamides in water. The simplification arises from the use of commercial, standardised reaction hardware which enables the polymerisations to be performed in a 2-electrode, ‘plug-n-play’, undivided electrochemical cell configuration. Further simplification is afforded by the design of a single stepwise current profile (Iapp vs time) capable of mediating current controlled eATRP of N-hydroethylacrylamide (HEAm). At room temperature, polymerisation of HEAm to target degrees of polymerisation (DPn,th¬) of 20 – 100 proceeds with good control (Ɖ ≤ 1.50). Loss of control when targeting higher DPn at room temperature is circumvented by lowering the reaction temperature (r.t. to 0 °C), increasing the stirring rate (400 rpm to 800 rpm) and increasing the catalyst concentration. Using the best conditions a linear increase in Mn,SEC with DPn (up to DPn = 320) and low dispersity values (DPn,th = 40 – 160; Ɖ = 1.26 – 1.38) are obtained. Furthermore, the current profile and reaction conditions can support the polymerisation of other primary and secondary acrylamides and the retention of the ω-Br chain end is exemplified by a short in situ chain extension. Overall, this represents further simplification of aqueous eATRP with respect to reaction set up and experimental parameters (single current profile) which has been employed synthesise polyacrylamides with good efficiency and control.
| Item Type: | Journal Article | |||||||||
|---|---|---|---|---|---|---|---|---|---|---|
| Subjects: | Q Science > QD Chemistry | |||||||||
| Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | |||||||||
| Library of Congress Subject Headings (LCSH): | Polymers, Polymerization, Free radical reactions, Macromolecules, Electrochemistry -- Research | |||||||||
| Journal or Publication Title: | Polymer Chemistry | |||||||||
| Publisher: | Royal Society of Chemistry | |||||||||
| ISSN: | 1759-9954 | |||||||||
| Official Date: | 21 June 2022 | |||||||||
| Dates: |
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| Volume: | 13 | |||||||||
| Number: | 23 | |||||||||
| Page Range: | pp. 3460-3470 | |||||||||
| DOI: | 10.1039/D2PY00412G | |||||||||
| Status: | Peer Reviewed | |||||||||
| Publication Status: | Published | |||||||||
| Access rights to Published version: | Open Access (Creative Commons) | |||||||||
| Date of first compliant deposit: | 18 May 2022 | |||||||||
| Date of first compliant Open Access: | 18 May 2022 | |||||||||
| RIOXX Funder/Project Grant: |
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