Synthesis and characterization of the layered sodium silicate ilerite

Abstract

A sodium ilerite, molar ratios 1Na 2O:8.2SiO 2:10.2H 2O, was obtained with a good crystalline structure and characterized by several NMR techniques in addition to X-ray diffraction (XRD). The X-ray pattern of the as-synthesized ilerite is in very good agreement with the structure proposed by Gies and coworkers. The narrow 29Si MAS NMR signals (FWHM=0.3 ppm) indicate a good short-range order of the framework. The proton dynamics influences several 29Si NMR parameters. The 16 ppm signal in the 1H MAS NMR spectra is explained by a proton in a bridging position in the short (2.3 Å) O4–O4 bonding. The quadrupole coupling constant C qcc=100 kHz with η=0.2 for the 16 ppm signal, which was obtained from the 2H MAS NMR spectra, confirms this explanation. 17O NMR shows also a separate signal for SiOH groups but cannot resolve the three expected lines for SiOSi. PFG NMR detects a small mobile portion of water in the ilerite, which is located probably on the external surface of the crystallites. An intracrystalline diffusion coefficient of the intercalated water molecules of the order of magnitude 10 −15 m 2 s −1 was obtained by NMR tracer exchange experiments.