radical polymerization; nitroxide-mediated polymerization (NMP); green technology; supercritical carbon dioxide
Abstract :
[en] Controlled dispersion Nitroxide Mediated Polymerization (NMP) of methyl methacrylate (MMA) was successfully carried out for the first time in supercritical carbon dioxide (scCO2) in the presence of CO2-philic perfluorinated surfactant that was generated “in situ”. The control of the MMA polymerization relies on the strategy developed by Charleux et al. that consists of using a SG1-based alkoxyamine, i.e. the block-builder, in the presence of small amount of styrene. In a first step, CO2 soluble polyheptadecafluorodecylacrylate was prepared in scCO2 using block-builder as an alkoxyamine. In a second step, nitroxide SG1 mediated dispersion polymerization of MMA was conducted at 70°C and 300 bar in the presence of 5 w% of SG1 terminated surfactant compared to the monomer. Different monomer to alkoxyamine molar ratios were investigated in order to target different molecular weights. In each case, the monomer conversion was high (>90 %), the experimental molecular weight was in good agreement with the theoretical value and the polydispersity was narrow (Mw/Mn ~1.2). Moreover, after depressurisation of the cell, PMMA was collected as a free flowing powder consisting of small sized microspheres.
Research Center/Unit :
Center for Education and Research on Macromolecules (CERM)
Disciplines :
Chemistry Materials science & engineering
Author, co-author :
Grignard, Bruno ; Université de Liège - ULiège > Department of Chemistry > Center for Education and Research on Macromolecules (CERM)
Gigmes, Didier; Universités d'Aix-Marseille 1, 2 et 3-CNRS, France > Chimie, Biologie et Radicaux Libres
Jérôme, Christine ; Université de Liège - ULiège > Department of Chemistry > Center for Education and Research on Macromolecules (CERM)
Detrembleur, Christophe ; Université de Liège - ULiège > Department of Chemistry > Center for Education and Research on Macromolecules (CERM)
Language :
English
Title :
In situ formation of stabilizers for the implementation of dispersion nitroxide mediated polymerization of MMA in supercritical carbon dioxide
Publication date :
17 September 2009
Event name :
Meeting on Controlled Radical Polymerization (CRP Meeting 2009) "Controlled/Living Radical Polymerizations: Latest trends in Synthesis, Characterization and Industrial Applications"
Event organizer :
P. Dubois, F. Du Prez, C. Barner-Kowolik
Event place :
Houffalize, Belgium
Event date :
17/09/2009 - 18/09/2009
Audience :
International
Funders :
F.R.S.-FNRS - Fonds de la Recherche Scientifique BELSPO - SPP Politique scientifique - Service Public Fédéral de Programmation Politique scientifique The "Région Wallonne" and the FEDER in the frame of the "SINOPLISS" project
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