Manning, J.R.H., Brambila, C., Rishi, K. et al. (3 more authors) (2024) Quality-by-design approach to process intensification of bioinspired silica synthesis. ACS Sustainable Chemistry & Engineering, 12 (12). pp. 4900-4911. ISSN 2168-0485
Abstract
Characterizing nanomaterials is challenging due to their macromolecular nature, requiring suites of physicochemical analysis to fully resolve their structure. As such, their synthesis and scale-up are notoriously complex, especially when compared to small molecules or bulk crystalline materials, which can be provided a unique fingerprint from nuclear magnetic resonance (NMR) or X-ray diffraction (XRD) alone. In this study, we address this challenge by adopting a three-step quality-by-design (QbD) approach to the scale-up of bioinspired silica nanomaterials, demonstrating its utility toward synthesis scale-up and intensification for this class of materials in general. First, we identified material-specific surface area, pore-size distribution, and reaction yield as critical quality attributes (CQAs) that could be precisely measured and controlled by changing reaction conditions. We then identified the critical process parameters (CPPs) controlling bioinspired synthesis properties, exploring different process routes, incorporating commercial reagents, and optimizing reagent ratios, comparing silica properties against original CQA values to identify acceptable limits to each CPP. Finally, we intensified the synthesis by increasing reagent concentration while simultaneously incorporating the optimized CPPs, thereby modifying the bioinspired silica synthesis to make it compatible with existing manufacturing methods. We increased the specific yield from ca. 1.1 to 38 g/L and reduced the additive intensity from ca. 1 to 0.04 g/g product, greatly reducing both synthesis cost and waste production. These results identify a need for mapping the effects of critical process parameters on material formation pathways and CQAs to enable accelerated scale-up and transition from the lab to the market.
Metadata
Item Type: | Article |
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Authors/Creators: |
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Copyright, Publisher and Additional Information: | © 2024 The Author(s). Published by American Chemical Society. This publication is licensed under CC-BY 4.0. (https://creativecommons.org/licenses/by/4.0/) |
Keywords: | manufacturing; scale-up; green chemistry; sustainability |
Dates: |
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Institution: | The University of Sheffield |
Academic Units: | The University of Sheffield > Faculty of Engineering (Sheffield) > Department of Chemical and Biological Engineering (Sheffield) |
Funding Information: | Funder Grant number ENGINEERING AND PHYSICAL SCIENCE RESEARCH COUNCIL EP/R025983/1 ENGINEERING AND PHYSICAL SCIENCE RESEARCH COUNCIL EP/P006892/1 ENGINEERING AND PHYSICAL SCIENCE RESEARCH COUNCIL EP/V051458/1 |
Depositing User: | Symplectic Sheffield |
Date Deposited: | 28 Feb 2024 14:49 |
Last Modified: | 02 Apr 2024 12:21 |
Status: | Published |
Publisher: | American Chemical Society |
Refereed: | Yes |
Identification Number: | 10.1021/acssuschemeng.3c07624 |
Open Archives Initiative ID (OAI ID): | oai:eprints.whiterose.ac.uk:209481 |