A replicated investigation of nitroxide-mediated radical polymerization of styrene over a range of reaction conditions

Authors

  • Afsaneh Nabifar,

    1. Department of Chemical Engineering, Institute for Polymer Research (IPR), University of Waterloo, Waterloo, Ontario, Canada N2L 3G1
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  • Neil T. McManus,

    1. Department of Chemical Engineering, Institute for Polymer Research (IPR), University of Waterloo, Waterloo, Ontario, Canada N2L 3G1
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  • Eduardo Vivaldo-Lima,

    1. Facultad de Química, Departamento de Ingeniería Química, Universidad Nacional Autónoma de México (UNAM), Conjunto E, Ciudad Universitaria, México CP 04510, D.F., Mexico
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  • Liliane M.F. Lona,

    1. Department of Chemical Processes, School of Chemical Engineering, State University of Campinas (UNICAMP), P.O. Box 6066, Campinas, São Paulo, Brazil
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  • Alexander Penlidis

    Corresponding author
    1. Department of Chemical Engineering, Institute for Polymer Research (IPR), University of Waterloo, Waterloo, Ontario, Canada N2L 3G1
    • Department of Chemical Engineering, Institute for Polymer Research (IPR), University of Waterloo, Waterloo, Ontario, Canada N2L 3G1.
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  • A. Penlidis dedicates this paper to Professor John F. MacGregor, who taught him how to appreciate process data. Thank you, JFM

Abstract

A comprehensive experimental investigation of nitroxide-mediated radical polymerization (NMRP) of styrene using 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) as controller is presented. Polymerizations with a bimolecular initiator (benzoyl peroxide; BPO) were carried out at 120 and 130°C, with TEMPO/BPO molar ratios ranging from 0.9 to 1.5. Results indicate that increasing temperature increases the rate of polymerization while the decrease in molecular weights is only slight. It was also observed that increasing the ratio of TEMPO/BPO decreased both the rate of polymerization and molecular weights. Probably for the first time in the history of such investigations, the paper contains a comprehensive database, appropriate for parameter estimation in aid of future modelling studies, since it comes from a systematic data collection containing independent replication.

Abstract

On présente une étude expérimentale approfondie de la polymérisation radicalaire basée sur les nitroxydes (NMRP) du styrène à l'aide de tétraméthyl-2,2,6,6 pipéridinyloxy-1 (TEMPO) comme agent de contrôle. Des polymérisations à l'aide d'un initiateur bimoléculaire (peroxyde de benzoyle, BPO) ont été menées à 120 et 130°C, avec des rapports molaires de TEMPO/BPO variant entre 0,9 à 1,5. Les résultats indiquent que l'augmentation de température accroît la vitesse de polymérisation tandis que la baisse des masses moléculaires n'est que légère. On a également observé que l'augmentation du rapport de TEMPO/BPO diminue à la fois la vitesse de polymérisation et les masses moléculaires. Probablement pour la première fois dans l'histoire de ce type de recherches, l'article contient une base de données complète, convenant à l'estimation de paramètres en vue d'études de modélisation futures, étant issue d'une collecte de données systématique.

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