Pittaway, P.M. orcid.org/0000-0003-2302-9263, Knox, S.T., Cayre, O.J. orcid.org/0000-0003-1339-3686 et al. (4 more authors) (2025) Self-driving laboratory for emulsion polymerization. Chemical Engineering Journal, 507. 160700. ISSN 1385-8947
Abstract
Modern approaches to chemical product discovery are exploiting the benefits of flow-chemistry, online characterization, and smart automation to rapidly screen and optimize chemical transformations. The present work describes the development and application of an automated continuous-flow reactor platform for the rapid prototyping of latexes prepared via seeded free-radical emulsion polymerization. Using a multi-reactor system comprising a cascade of miniature continuous stirred-tank reactors (CSTRs) followed by a sonicated tubular reactor (STR) with five pumps for reagent delivery, the capability to explore a four-dimensional parameter space of surfactant concentration, seed fraction, monomer ratio, and feed-rate is demonstrated. With user-defined boundary conditions, a one-factor-at-a-time (OFAAT) approach first illustrates the capability to prepare products with unique and tuneable properties. Subsequently, an experimental design is constructed to explore a three-dimensional parameter space, with 16 reactions completed in under three days of platform time. This rapid generation of product prototypes allowed features of the polymer system to be evaluated on a timescale much shorter than traditional methods with a significant reduction in manual effort and human-chemical interaction. The resulting response surface model was applied for in silico optimization using the Thompson-sampling efficient multi-objective (TSEMO) optimization algorithm. Finally, online dynamic light scattering (DLS) was applied with the physical platform which enabled self-optimization of the polymerization, identifying the attainable particle sizes whilst minimizing the amounts of seed and surfactant used. Closing the loop resulted in a fully operational self-driving laboratory.
Metadata
Item Type: | Article |
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Authors/Creators: |
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Copyright, Publisher and Additional Information: | © 2025 The Authors. This is an open access article under the terms of the Creative Commons Attribution License (CC-BY 4.0), which permits unrestricted use, distribution and reproduction in any medium, provided the original work is properly cited. |
Dates: |
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Institution: | The University of Leeds |
Academic Units: | The University of Leeds > Faculty of Engineering & Physical Sciences (Leeds) > School of Chemical & Process Engineering (Leeds) The University of Leeds > Faculty of Engineering & Physical Sciences (Leeds) > School of Mechanical Engineering (Leeds) |
Depositing User: | Symplectic Publications |
Date Deposited: | 28 May 2025 15:12 |
Last Modified: | 28 May 2025 15:12 |
Status: | Published |
Publisher: | Elsevier |
Identification Number: | 10.1016/j.cej.2025.160700 |
Open Archives Initiative ID (OAI ID): | oai:eprints.whiterose.ac.uk:227090 |