Issue 3, 2023

Continuous synthesis of block copolymer nanoparticles via telescoped RAFT solution and dispersion polymerisation in a miniature CSTR cascade

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.

Graphical abstract: Continuous synthesis of block copolymer nanoparticles via telescoped RAFT solution and dispersion polymerisation in a miniature CSTR cascade

Supplementary files

Article information

Article type
Paper
Submitted
07 nov 2022
Accepted
09 dec 2022
First published
12 dec 2022
This article is Open Access
Creative Commons BY license

React. Chem. Eng., 2023,8, 707-717

Continuous synthesis of block copolymer nanoparticles via telescoped RAFT solution and dispersion polymerisation in a miniature CSTR cascade

P. M. Pittaway, G. Ghasemi, S. T. Knox, O. J. Cayre, N. Kapur and N. J. Warren, React. Chem. Eng., 2023, 8, 707 DOI: 10.1039/D2RE00475E

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