Characterization of Polyalkylvinyl Ether Phases by Solid-State and Suspended-State Nuclear Magnetic Resonance Investigations

Abstract

Pure organic polyalkylvinyl ether phases were synthesized by suspension polymerization using different ratios and compositions of n-butylvinyl ether (C4VE) and n-octadecylvinyl ether (C18VE) with triethylene glycol divinyl ether or divinylbenzene as crosslinkers, respectively. These phases were investigated by means of solid-state 13C cross-polarization magic angle spinning nuclear magnetic resonance (NMR) spectroscopy and 1H high-resolution magic angle spinning (HR MAS) NMR spectroscopy in suspended-state. A comparison of these two methods showed the substantial advantages of 1H HR MAS NMR measurements. Structure elucidation was achieved using a 2D H,H-COSY NMR experiment performed under MAS conditions enabling full peak assignment of the 1H NMR spectra of these phases. The dynamic behavior of the polyalkylvinyl ether phases was determined by employing temperature-dependent measurements of spin–lattice relaxation times (T1) as well as accumulation of a 2D wide line separation NMR spectrum.