Star polymer with crosslinked core and water-soluble poly(N- hydroxyethylacrylamide)-arms: Synthesis by arm-first method using ATRP and characterizations by SEC-MALS and SAXS measurement in water

Atsushi Narumi, Yoko Ohashi, Daichi Togashi, Yuta Saito, Yuji Jinbo, Yoshinobu Izumi, Keigo Matsuda, Toyoji Kakuchi, Seigou Kawaguchi

Research output: Contribution to journalArticle

5 Citations (Scopus)

Abstract

Core crosslinked star (CCS)-polymers with water-soluble arms composed of poly(N-hydroxyethylacrylamide) (PHEAA) are described. N-Hydroxyethylacrylamide was polymerized by the atom transfer radical polymerization consisting of ethyl 2-chloropropionate, copper(I) chloride (CuCl), and tris[2-(dimethylamino)ethyl] amine in an ethanol/water mixed solvent at 20 °C. The obtained PHEAA-arms were subsequently coupled using N,N'-methylenebisacrylamide as the crosslinking agent and sodium L-ascorbic acid (AscNa) as the reaction activator. A total of 17 representative coupling reactions with diverse conditions are discussed together with the characterizations of the products mainly by size exclusion chromatograph equipped with the multiangle laser light scattering detector (SEC-MALS). Consequently, the coupling reactions provided CCS-polymers with PHEAA-arms (CCS-PHEAAs) having weight averaged-molecular weights determined by SEC-MALS (M w,MALS) ranging from 63.8 kg mol -1 to 832 kg mol -1, which corresponded to the average arm-number (N arm) ranging from 4.1 to 42, respectively. CCS-PHEAA with the M w,MALS of 250 kg mol -1 was isolated and characterized by small angle X-ray scattering measurements in 0.05 M NaNO 3 aq. at 25 °C, which was shown to possess a star-shaped structure and exist as single molecules with a radius of gyration at the infinite dilution condition (<R g 2> z,0 1/2) of 74 ± 4 Å.

Original languageEnglish
Pages (from-to)3546-3559
Number of pages14
JournalJournal of Polymer Science, Part A: Polymer Chemistry
Volume50
Issue number17
DOIs
Publication statusPublished - 2012 Sep 1

Keywords

  • SAXS
  • atom transfer radical polymerization (ATRP)
  • solution properties
  • star polymers
  • water-soluble polymers

ASJC Scopus subject areas

  • Polymers and Plastics
  • Organic Chemistry
  • Materials Chemistry

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