Copper-mediated homogeneous living radical polymerization of acrylamide with waxy potato starch-based macroinitiator

Yifei Fan; Huatang Cao; Frank van Mastrigt; Yutao Pei; Francesco Picchioni

doi:10.1016/j.carbpol.2018.03.041

Copper-mediated homogeneous living radical polymerization of acrylamide with waxy potato starch-based macroinitiator

Carbohydr Polym. 2018 Jul 15:192:61-68. doi: 10.1016/j.carbpol.2018.03.041. Epub 2018 Mar 15.

Authors

Yifei Fan¹, Huatang Cao², Frank van Mastrigt¹, Yutao Pei², Francesco Picchioni³

Affiliations

¹ Department of Chemical Engineering, Engineering and Technology Institute Groningen, University of Groningen, Nijenborgh 4, 9747AG Groningen, The Netherlands.
² Department of Advanced Production Engineering, Engineering and Technology Institute Groningen, University of Groningen, Nijenborgh 4, 9747AG Groningen, The Netherlands.
³ Department of Chemical Engineering, Engineering and Technology Institute Groningen, University of Groningen, Nijenborgh 4, 9747AG Groningen, The Netherlands. Electronic address: f.picchioni@rug.nl.

PMID: 29691035
DOI: 10.1016/j.carbpol.2018.03.041

Abstract

Cu⁰-mediated living radical polymerization (Cu⁰-mediated LRP) was employed in this research for the synthesis of starch-g-polyacrylamide (St-g-PAM). The use of a controlled radical grafting technique is necessary, as compared to the traditional free-radical polymerization methods, in order to obtain a well-defined structure of the final product. This is in turn essential for studying the relationship between such structure and the end-properties. Waxy potato starch-based water-soluble macroinitiator was first synthesized by esterification with 2-bromopropionyl bromide in the mixture of dimethylacetamide and lithium chloride. With the obtained macroinitiator, St-g-PAM was homogeneously synthesized by aqueous Cu⁰-mediated LRP using CuBr/hexamethylated tris(2-aminoethyl)amine (Me₆Tren) as catalyst. The successful synthesis of the macroinitiator and St-g-PAM was proved by NMR, FT-IR, SEM, XRD and TGA analysis. The molecular weight and polydispersity of PAM chains were analyzed by gel permeation chromatography (GPC) after hydrolyzing the starch backbone. Monomer conversion was monitored by gas chromatography (GC), on the basis of which the kinetics were determined. A preliminarily rheological study was performed on aqueous solutions of the prepared materials.

Keywords: Cu(0)-mediated living radical polymerization; Graft; Homogeneous; Polyacrylamide; Waxy potato starch.