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Solid‐State NMR Spectroscopic Studies of Propylphosphonic Acid Functionalized SBA‐15 Mesoporous Silica: Characterization of Hydrogen‐Bonding Interactions
Author(s) -
Bibent Nicolas,
Charpentier Thibault,
DevautourVinot Sabine,
Mehdi Ahmad,
Gaveau Philippe,
Henn François,
Silly Gilles
Publication year - 2013
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201201404
Subject(s) - chemistry , mesoporous material , solid state nuclear magnetic resonance , hydrogen bond , mesoporous silica , nuclear magnetic resonance spectroscopy , transmission electron microscopy , desorption , silanol , crystallography , adsorption , nanotechnology , molecule , organic chemistry , catalysis , nuclear magnetic resonance , materials science , physics
This work aims to investigate the local structure of mesoporous silica of the type SBA‐15 functionalized with propylphosphonic acid groups by means of an extensive solid‐state NMR spectroscopic study. Here, the functionalized SBA‐15 samples are obtained by a one‐step synthetic method that allowed us better control over the loading and the distribution of the surface functions. In addition to NMR spectroscopy, the materials are characterized by X‐ray diffraction, nitrogen adsorption–desorption and transmission electron microscopy. The 29 Si, 13 C, 31 P and 1 H one‐dimensional NMR spectroscopic results are discussed according to the nature of the functional groups in dry and wet materials. This paper proposes a rigorous approach that shows possible hydrogen bonding between adjacent phosphonic acid groups in dry SBA‐15, from the comparative study with an alkylphosphonic acid material. This outcome was demonstrated by two‐dimensional NMR spectroscopic solid–state experiments, including the use of 1 H– 1 H spin‐diffusion exchange experiments, 31 P– 31 P double quanta and an original pulse sequence that corresponds to 31 P– 1 H– 1 H– 31 P correlation experiments.