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Temperature Responsive Cellulose-graft-Copolymers via Cellulose Functionalization in an Ionic Liquid and RAFT Polymerization

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Preparative Macromolecular Chemistry, Institut für Technische Chemie und Polymerchemie, Karlsruhe Institute of Technology (KIT), Engesserstr. 18, 76128 Karlsruhe, Germany
Institut für Biologische Grenzflächen and Institute for Applied Materials (IAM) and Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology (KIT), Herrmann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
§ Laboratory of Applied Chemistry, Institute of Organic Chemistry, Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe, Germany
*E-mail: [email protected]; [email protected]. Web: www.macroarc.de; www.meier-michael.com.
Cite this: Biomacromolecules 2014, 15, 7, 2563–2572
Publication Date (Web):May 15, 2014
https://doi.org/10.1021/bm500416m
Copyright © 2014 American Chemical Society

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    Abstract

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    Well-defined cellulose-graft-polyacrylamide copolymers were synthesized in a grafting-from approach by reversible addition–fragmentation chain transfer polymerization (RAFT). A chlorine moiety (degree of substitution DS(Cl) ≈ 1.0) was introduced into the cellulose using 1-butyl-3-methylimidazolium chloride (BMIMCl) as solvent before being substituted by a trithiocarbonate moiety resulting in cellulose macro-chain transfer agents (cellulose-CTA) with DS(RAFT) of 0.26 and 0.41. Poly(N,N-diethylacrylamide) (PDEAAm) and poly(N-isopropylacrylamide) (PNIPAM) were subsequently grafted from these cellulose-CTAs and the polymerization kinetics, the molecular weight characteristics and the product composition were studied by nuclear magnetic resonance spectroscopy, X-ray photoelectron spectroscopy, and size exclusion chromatography of the polyacrylamides after cleavage from the cellulose chains. The number-average molecular weights, Mn, of the cleaved polymers ranged from 1100 to 1600 g mol–1 for PDEAAm (dispersity Đ = 1.4–1.8) and from 1200 to 2600 g mol –1 for PNIPAM (Đ = 1.7–2.1). The LCST behavior of the cellulose-graft-copolymers was studied via the determination of cloud point temperatures, evidencing that the thermoresponsive properties of the hybrid materials could be finely tuned between 18 and 26 °C for PDEAAm and between 22 and 26 °C for PNIPAM side chains.

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    Additional SEC, NMR, and XPS data as well as additional information on thermoresponsive behavior. This material is available free of charge via the Internet at http://pubs.acs.org.

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