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Homogeneous phase polymerization of vinylidene fluoride in supercritical carbon dioxide
Authors:Sabine Beuermann  Muhammad Imran‐ul‐Haq
Affiliation:1. Institute of Chemistry, University of Potsdam, D 14476 Golm/Potsdam, GermanyInstitute of Chemistry, University of Potsdam, D 14476 Golm/Potsdam, Germany;2. Institute of Chemistry, University of Potsdam, D 14476 Golm/Potsdam, Germany
Abstract:For the first time, stabilizer‐free vinylidene fluoride (VDF) homopolymerizations were carried out in homogenous phase with supercritical CO2 using the conventional initiator di‐tert butyl peroxide (DTBP). In‐line FT‐NIR spectroscopy showed that complete monomer conversion may be obtained. Molecular weights were determined via size‐exclusion chromatography and polymer endgroup analysis by 1H‐NMR spectroscopy. The number average molecular weights were below 104 g mol?1 and polydispersities ranged from 3.1 to 5.7 depending on DTBP and VDF concentration. For allowing isothermal reaction, high CO2 contents ranging from 61 to 83 wt % were used. The high‐temperature and high‐pressure conditions required for homogeneous polymerization did not alter the amount of defects in VDF chaining. Scanning electron microscopy indicated that regular stack‐type particles are obtained upon expansion of the homogeneous polymerization mixture. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 5626–5635, 2007
Keywords:fluoropolymers  FT‐NIR  homogeneous phase  radical polymerization  supercritical carbon dioxide  vinylidene fluoride
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