Pittaway, P.M. orcid.org/0000-0003-2302-9263, Ghasemi, G., Knox, S.T. orcid.org/0000-0001-5276-0085 et al. (3 more authors) (2022) Continuous synthesis of block copolymer nanoparticles via telescoped RAFT solution and dispersion polymerisation in a miniature CSTR cascade. Reaction Chemistry & Engineering, 8 (3). pp. 707-717. ISSN 2058-9883
Abstract
Miniaturised continuous-flow reactors offer a safe, economical, and scalable route to explore the synthesis of high-value chemical products. In the context of polymer synthesis, precisely defined and tuneable products can be prepared via reversible de-activation radical polymerisation (RDRP) techniques such as reversible addition-fragmentation chain-transfer (RAFT), for which tubular reactors are commonly reported. Herein, we present a miniature continuous stirred-tank reactor (CSTR) cascade for continuous-flow RAFT polymerisation with active mixing throughout, which is found to perform close to a theoretical CSTR cascade for the polymerisations considered in this study. The performance of the reactor is evaluated for both the aqueous solution RAFT polymerisation of N,N-dimethylacrylamide (DMAm) and the RAFT dispersion polymerisation of diacetone acrylamide using a poly(DMAm) macromolecular chain transfer agent (macro-CTA). It was determined that the residence time distribution (RTD) is important for informing the properties of the resulting polymers, with more CSTRs resulting in a narrower molar mass distribution. For particle synthesis by polymerisation-induced self-assembly (PISA), a series of block copolymers were prepared in separate batch and flow experiments for which the particles obtained were found to vary despite comparable molecular weights. Towards the development of a high throughput screening platform, a multi-stage, telescoped tubular-CSTR cascade reactor configuration was applied for inline macro-CTA synthesis and subsequent block extension. Differences in product properties between the processing methods used supports the idea that polymers are so-called ‘products-by-process’; indeed different polymer products can be accessed from the same chemistry through the application of alternative synthesis approaches.
Metadata
Item Type: | Article |
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Authors/Creators: |
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Copyright, Publisher and Additional Information: | © The Royal Society of Chemistry 2023. This article is licensed under a Creative Commons Attribution 3.0 Unported Licence. https://creativecommons.org/licenses/by/3.0/ |
Keywords: | Macromolecular and Materials Chemistry; Engineering; Chemical Sciences |
Dates: |
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Institution: | The University of Sheffield |
Academic Units: | The University of Sheffield > Faculty of Engineering (Sheffield) > Department of Materials Science and Engineering (Sheffield) |
Funding Information: | Funder Grant number Engineering and Physical Sciences Research Council EP/V055089/1 |
Depositing User: | Symplectic Sheffield |
Date Deposited: | 09 Aug 2024 15:30 |
Last Modified: | 09 Aug 2024 15:30 |
Status: | Published |
Publisher: | Royal Society of Chemistry (RSC) |
Refereed: | Yes |
Identification Number: | 10.1039/d2re00475e |
Related URLs: | |
Open Archives Initiative ID (OAI ID): | oai:eprints.whiterose.ac.uk:215743 |