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 1H 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 1H resonances in aminopropyl-modified SBA matrix and notably allows the assignment of the protons resonance of the amino group.

Solid state NMR characterization of phenylphosphonic acid encapsulated in SBA-15 and aminopropyl-modified SBA-15

TESTA, Flaviano;
2013

Abstract

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 1H 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 1H resonances in aminopropyl-modified SBA matrix and notably allows the assignment of the protons resonance of the amino group.
Mesoporous Materials; Silica; Encapsulation
File in questo prodotto:
Non ci sono file associati a questo prodotto.

I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/20.500.11770/156913
 Attenzione

Attenzione! I dati visualizzati non sono stati sottoposti a validazione da parte dell'ateneo

Citazioni
  • ???jsp.display-item.citation.pmc??? ND
  • Scopus 40
  • ???jsp.display-item.citation.isi??? 22
social impact