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Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE)

Despite the great potential of design of experiments (DoE) for efficiency and plannability in academic research, it remains a method predominantly used in industrial processes. From our perspective though, DoE additionally provides greater information gain than conventional experimentation approache...

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Autores principales: Eckert, Tilman, Klein, Florian C., Frieler, Piet, Thunich, Oliver, Abetz, Volker
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2021
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8468855/
https://www.ncbi.nlm.nih.gov/pubmed/34578048
http://dx.doi.org/10.3390/polym13183147
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author Eckert, Tilman
Klein, Florian C.
Frieler, Piet
Thunich, Oliver
Abetz, Volker
author_facet Eckert, Tilman
Klein, Florian C.
Frieler, Piet
Thunich, Oliver
Abetz, Volker
author_sort Eckert, Tilman
collection PubMed
description Despite the great potential of design of experiments (DoE) for efficiency and plannability in academic research, it remains a method predominantly used in industrial processes. From our perspective though, DoE additionally provides greater information gain than conventional experimentation approaches, even for more complex systems such as chemical reactions. Hence, this work presents a comprehensive DoE investigation on thermally initiated reversible addition–fragmentation chain transfer (RAFT) polymerization of methacrylamide (MAAm). To facilitate the adaptation of DoE for virtually every other polymerization, this work provides a step-by-step application guide emphasizing the biggest challenges along the way. Optimization of the RAFT system was achieved via response surface methodology utilizing a face-centered central composite design (FC-CCD). Highly accurate prediction models for the responses of monomer conversion, theoretical and apparent number averaged molecular weights, and dispersity are presented. The obtained equations not only facilitate thorough understanding of the observed system but also allow selection of synthetic targets for each individual response by prediction of the respective optimal factor settings. This work successfully demonstrates the great capability of DoE in academic research and aims to encourage fellow scientists to incorporate the technique into their repertoire of experimental strategies.
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spelling pubmed-84688552021-09-27 Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE) Eckert, Tilman Klein, Florian C. Frieler, Piet Thunich, Oliver Abetz, Volker Polymers (Basel) Article Despite the great potential of design of experiments (DoE) for efficiency and plannability in academic research, it remains a method predominantly used in industrial processes. From our perspective though, DoE additionally provides greater information gain than conventional experimentation approaches, even for more complex systems such as chemical reactions. Hence, this work presents a comprehensive DoE investigation on thermally initiated reversible addition–fragmentation chain transfer (RAFT) polymerization of methacrylamide (MAAm). To facilitate the adaptation of DoE for virtually every other polymerization, this work provides a step-by-step application guide emphasizing the biggest challenges along the way. Optimization of the RAFT system was achieved via response surface methodology utilizing a face-centered central composite design (FC-CCD). Highly accurate prediction models for the responses of monomer conversion, theoretical and apparent number averaged molecular weights, and dispersity are presented. The obtained equations not only facilitate thorough understanding of the observed system but also allow selection of synthetic targets for each individual response by prediction of the respective optimal factor settings. This work successfully demonstrates the great capability of DoE in academic research and aims to encourage fellow scientists to incorporate the technique into their repertoire of experimental strategies. MDPI 2021-09-17 /pmc/articles/PMC8468855/ /pubmed/34578048 http://dx.doi.org/10.3390/polym13183147 Text en © 2021 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Eckert, Tilman
Klein, Florian C.
Frieler, Piet
Thunich, Oliver
Abetz, Volker
Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE)
title Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE)
title_full Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE)
title_fullStr Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE)
title_full_unstemmed Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE)
title_short Experimental Design in Polymer Chemistry—A Guide towards True Optimization of a RAFT Polymerization Using Design of Experiments (DoE)
title_sort experimental design in polymer chemistry—a guide towards true optimization of a raft polymerization using design of experiments (doe)
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8468855/
https://www.ncbi.nlm.nih.gov/pubmed/34578048
http://dx.doi.org/10.3390/polym13183147
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