期刊
MICROPOROUS AND MESOPOROUS MATERIALS
卷 166, 期 -, 页码 109-116出版社
ELSEVIER
DOI: 10.1016/j.micromeso.2012.04.028
关键词
Mesoporous materials; Silica; Encapsulation; Phosphonic acid; Solid state NMR
We present in this communication that phenyl phosphonic acid can be efficiently loaded in mesoporous SBA-15 and aminopropyl-modified SBA powdered samples through the incipient wetness impregnation method. High amount of phosphonic acid can be reach up to 380 mg/g of sample. We use multinuclear solid state NMR as a method of choice for the indeep characterization of the samples. Thus we demonstrate that phosphonic acid molecules do not crystallize inside the pores. The molecules are highly mobile in SBA-15 because they are submitted to a confinement effect due to the mesoscopic size of the pores and consequently they exhibit a weak interaction with the silica walls. In the case of aminopropyl-modified SBA material, we show that the molecules are rigid and that they are in strong interaction with the aminopropyl groups. Moreover, a 2D double quantum H-1 NMR experiment recorded at high field and high spinning speed permit to propose a model of the phosphonate-aminopropyl interaction. The increase in spectral resolution due to the combination of high magnetic field and fast MAS rate allows also the assignment of H-1 resonances in aminopropyl-modified SBA matrix and notably allows the assignment of the protons resonance of the amino group. (C) 2012 Elsevier Inc. All rights reserved.
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