Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk
International audience Among the various catalysts that can be used for polycondensation reactions, enzymes have been gaining interest for three decades, offering a green and eco-friendly platform towards the sustainable design of renewable polyesters. However, limitations imposed by their delicate...
Published in: | Polymers |
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Format: | Article in Journal/Newspaper |
Language: | English |
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HAL CCSD
2020
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Online Access: | https://hal.univ-lille.fr/hal-03247367 https://hal.univ-lille.fr/hal-03247367/document https://hal.univ-lille.fr/hal-03247367/file/polymers-892901.pdf https://doi.org/10.3390/polym12091907 |
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ftunivlille:oai:HAL:hal-03247367v1 2024-06-23T07:45:42+00:00 Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk Nasr, Kifah Meimoun, Julie Favrelle-Huret, Audrey Winter, Julien De Raquez, Jean-Marie Zinck, Philippe Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS) Université d'Artois (UA)-Centrale Lille-Institut de Chimie - CNRS Chimie (INC-CNRS)-Université de Lille-Centre National de la Recherche Scientifique (CNRS) Université de Mons / University of Mons (UMONS) Centre d'Innovation et de Recherche en Matériaux Polymères (CIRMAP) 2020 https://hal.univ-lille.fr/hal-03247367 https://hal.univ-lille.fr/hal-03247367/document https://hal.univ-lille.fr/hal-03247367/file/polymers-892901.pdf https://doi.org/10.3390/polym12091907 en eng HAL CCSD MDPI info:eu-repo/semantics/altIdentifier/doi/10.3390/polym12091907 hal-03247367 https://hal.univ-lille.fr/hal-03247367 https://hal.univ-lille.fr/hal-03247367/document https://hal.univ-lille.fr/hal-03247367/file/polymers-892901.pdf doi:10.3390/polym12091907 info:eu-repo/semantics/OpenAccess ISSN: 2073-4360 Polymers https://hal.univ-lille.fr/hal-03247367 Polymers, 2020, 12 (9), pp.1907. ⟨10.3390/polym12091907⟩ enzymatic polymerization polycondensation lipase polyesters response surface methodology recyclability [CHIM.POLY]Chemical Sciences/Polymers info:eu-repo/semantics/article Journal articles 2020 ftunivlille https://doi.org/10.3390/polym12091907 2024-06-03T15:00:50Z International audience Among the various catalysts that can be used for polycondensation reactions, enzymes have been gaining interest for three decades, offering a green and eco-friendly platform towards the sustainable design of renewable polyesters. However, limitations imposed by their delicate nature, render them less addressed. As a case study, we compare herein bulk and solution polycondensation of 1,6-hexanediol and diethyl adipate catalyzed by an immobilized lipase from Candida antarctica. The influence of various parameters including time, temperature, enzyme loading, and vacuum was assessed in the frame of a two-step polymerization with the help of response surface methodology, a statistical technique that investigates relations between input and output variables. Results in solution (diphenyl ether) and bulk conditions showed that a two-hour reaction time was enough to allow adequate oligomer growth for the first step conducted under atmospheric pressure at 100 °C. The number-average molecular weight (Mn) achieved varied between 5000 and 12,000 g·mol−1 after a 24 h reaction and up to 18,500 g∙mol−1 after 48 h. The statistical analysis showed that vacuum was the most influential factor affecting the Mn in diphenyl ether. In sharp contrast, enzyme loading was found to be the most influential parameter in bulk conditions. Recyclability in bulk conditions showed a constant Mn of the polyester over three cycles, while a 17% decrease was noticed in solution. The following work finally introduced a statistical approach that can adequately predict the Mn of poly(hexylene adipate) based on the choice of parameter levels, providing a handy tool in the synthesis of polyesters where the control of molecular weight is of importance. Article in Journal/Newspaper Antarc* Antarctica LillOA (HAL Lille Open Archive, Université de Lille) Polymers 12 9 1907 |
institution |
Open Polar |
collection |
LillOA (HAL Lille Open Archive, Université de Lille) |
op_collection_id |
ftunivlille |
language |
English |
topic |
enzymatic polymerization polycondensation lipase polyesters response surface methodology recyclability [CHIM.POLY]Chemical Sciences/Polymers |
spellingShingle |
enzymatic polymerization polycondensation lipase polyesters response surface methodology recyclability [CHIM.POLY]Chemical Sciences/Polymers Nasr, Kifah Meimoun, Julie Favrelle-Huret, Audrey Winter, Julien De Raquez, Jean-Marie Zinck, Philippe Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk |
topic_facet |
enzymatic polymerization polycondensation lipase polyesters response surface methodology recyclability [CHIM.POLY]Chemical Sciences/Polymers |
description |
International audience Among the various catalysts that can be used for polycondensation reactions, enzymes have been gaining interest for three decades, offering a green and eco-friendly platform towards the sustainable design of renewable polyesters. However, limitations imposed by their delicate nature, render them less addressed. As a case study, we compare herein bulk and solution polycondensation of 1,6-hexanediol and diethyl adipate catalyzed by an immobilized lipase from Candida antarctica. The influence of various parameters including time, temperature, enzyme loading, and vacuum was assessed in the frame of a two-step polymerization with the help of response surface methodology, a statistical technique that investigates relations between input and output variables. Results in solution (diphenyl ether) and bulk conditions showed that a two-hour reaction time was enough to allow adequate oligomer growth for the first step conducted under atmospheric pressure at 100 °C. The number-average molecular weight (Mn) achieved varied between 5000 and 12,000 g·mol−1 after a 24 h reaction and up to 18,500 g∙mol−1 after 48 h. The statistical analysis showed that vacuum was the most influential factor affecting the Mn in diphenyl ether. In sharp contrast, enzyme loading was found to be the most influential parameter in bulk conditions. Recyclability in bulk conditions showed a constant Mn of the polyester over three cycles, while a 17% decrease was noticed in solution. The following work finally introduced a statistical approach that can adequately predict the Mn of poly(hexylene adipate) based on the choice of parameter levels, providing a handy tool in the synthesis of polyesters where the control of molecular weight is of importance. |
author2 |
Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS) Université d'Artois (UA)-Centrale Lille-Institut de Chimie - CNRS Chimie (INC-CNRS)-Université de Lille-Centre National de la Recherche Scientifique (CNRS) Université de Mons / University of Mons (UMONS) Centre d'Innovation et de Recherche en Matériaux Polymères (CIRMAP) |
format |
Article in Journal/Newspaper |
author |
Nasr, Kifah Meimoun, Julie Favrelle-Huret, Audrey Winter, Julien De Raquez, Jean-Marie Zinck, Philippe |
author_facet |
Nasr, Kifah Meimoun, Julie Favrelle-Huret, Audrey Winter, Julien De Raquez, Jean-Marie Zinck, Philippe |
author_sort |
Nasr, Kifah |
title |
Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk |
title_short |
Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk |
title_full |
Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk |
title_fullStr |
Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk |
title_full_unstemmed |
Enzymatic Polycondensation of 1,6-Hexanediol and Diethyl Adipate: A Statistical Approach Predicting the Key-Parameters in Solution and in Bulk |
title_sort |
enzymatic polycondensation of 1,6-hexanediol and diethyl adipate: a statistical approach predicting the key-parameters in solution and in bulk |
publisher |
HAL CCSD |
publishDate |
2020 |
url |
https://hal.univ-lille.fr/hal-03247367 https://hal.univ-lille.fr/hal-03247367/document https://hal.univ-lille.fr/hal-03247367/file/polymers-892901.pdf https://doi.org/10.3390/polym12091907 |
genre |
Antarc* Antarctica |
genre_facet |
Antarc* Antarctica |
op_source |
ISSN: 2073-4360 Polymers https://hal.univ-lille.fr/hal-03247367 Polymers, 2020, 12 (9), pp.1907. ⟨10.3390/polym12091907⟩ |
op_relation |
info:eu-repo/semantics/altIdentifier/doi/10.3390/polym12091907 hal-03247367 https://hal.univ-lille.fr/hal-03247367 https://hal.univ-lille.fr/hal-03247367/document https://hal.univ-lille.fr/hal-03247367/file/polymers-892901.pdf doi:10.3390/polym12091907 |
op_rights |
info:eu-repo/semantics/OpenAccess |
op_doi |
https://doi.org/10.3390/polym12091907 |
container_title |
Polymers |
container_volume |
12 |
container_issue |
9 |
container_start_page |
1907 |
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1802641952522371072 |