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Journal of Polymer Research

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01.08.2021 | ORIGINAL PAPER

Radical polymerization of butadiene mediated by molecular iodine: a kinetic study of solution homopolymerization

verfasst von: Mahdi Abdollahi, Masoud Akbari Hajiataloo

Erschienen in: Journal of Polymer Research | Ausgabe 8/2021

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Abstract

Homopolymerization of butadiene (Bu) in 1,4-dioxane (Dox) was performed at 70 °C using molecular iodine (I₂) in the presence of 4,4’-azobis(4-cyanovaleric acid) (ACVA), resulting in α-carboxyl ω-iodine heterotelechelic polybutadiene. Effect of Dox concentration, molar ratio of ACVA to I₂ and initiator type on the Bu conversion was studied. Inhibition of the reaction by molecular I₂ was observed until complete consumption of the I₂ (induction period). Then, polymerization initiated by carboxyl- functionalized alkyl iodides in situ generated during induction period. ACVA decomposition rate constant (k_d), induction time \(\left({t}_{ind}\right)\) and \({k}_{p}^{2}/{k}_{t}\) ratio were calculated using Bu conversion as a function of time data. A good agreement between the theoretical and experimental changes in the conversion versus time was observed, indicating accuracy of the kinetic parameters estimated in this work. Experimental \({t}_{ind}\) was always less that theoretical one. It was attributed to reaction between Bu and I₂, resulting in butadiene diiodide (I-Bu-I) compound. Formation of I-Bu-I species was further confirmed by ¹H-NMR analysis of end functional groups (i.e. alkyl iodide and allyl iodide) of polybutadiene chains. Based on the ¹H-NMR analysis, [I-Bu-I]/[I₂]₀ ratio was obtained for reaction B4 to be 0.235. It was found that among 1,2 and 1,4 additions, 1,2 addition of I₂ to Bu is the dominant reaction. Exchange constant between the growing and dormant species (C_ex) was estimated using GPC and conversion data to be in the range of 3.20–3.94. Then, \({M}_{n}\) and \(D\) evolution with conversion was investigated theoretically. Fraction of \(\alpha -\) carboxyl, \(\omega-\) iodide heterotelechelic PBu chains \(\left({f}_{HOOC-PBu-I}\right)\) relative to all chains was estimated from ¹H-NMR data to be 87% for reaction B4.

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Titel: Radical polymerization of butadiene mediated by molecular iodine: a kinetic study of solution homopolymerization
verfasst von: Mahdi Abdollahi
Masoud Akbari Hajiataloo
Publikationsdatum: 01.08.2021
Verlag: Springer Netherlands
Erschienen in: Journal of Polymer Research / Ausgabe 8/2021
Print ISSN: 1022-9760
Elektronische ISSN: 1572-8935
DOI: https://doi.org/10.1007/s10965-021-02617-8

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