Inour previous study we reported that is possible to perform the intercalation of phenylbenzimidazolsulfonic-acid into (Milanesio et al.) layered double hydroxide materials (LDH) exploiting an easy and fast solid state reaction. In this paper this method for the preparation of exchanged LDHs was extended to other compounds with different chemical features. Moreover the fast in situ X-ray powder diffraction measurements, performed using synchrotron radiation, allowed to unravel the mechanism and kinetics of the process. This showed that it is possible to carry out the reaction in less than 1000 sec instead of days. The chosen organic guests were 3-carboxy coumarin and, given their importance, a series of non-steroidal anti-inflammatory drugs with different pKa values and steric hindrance; namely ketoprofen, flurbiprofen, ibuprofen, indomethacin and tiaprofenic acid. The method has been applied to different classes of compounds to characterize the reaction in terms of speed, yield and also applicability. The characterization of the obtained nano-composites, carried out by crystallographic and microscopic techniques, revealed that the synthesis yield is comparable to that of standard methods, but with enormous time, solvent, and energy saving advantages. Moreover, the in situ diffraction experiments allowed to shed some light on the kinetics of the intercalation process with sub-second resolution and to determine the parameters affecting the reaction. Steric hindrance of the molecule proved to be the most relevant parameter to de-termine the applicability of this method. Finally we also show that our method can be easily up scaled.

Development of fast and clean intercalation method for organic molecules into layered double hydroxides.

PERIOLI, Luana;
2013

Abstract

Inour previous study we reported that is possible to perform the intercalation of phenylbenzimidazolsulfonic-acid into (Milanesio et al.) layered double hydroxide materials (LDH) exploiting an easy and fast solid state reaction. In this paper this method for the preparation of exchanged LDHs was extended to other compounds with different chemical features. Moreover the fast in situ X-ray powder diffraction measurements, performed using synchrotron radiation, allowed to unravel the mechanism and kinetics of the process. This showed that it is possible to carry out the reaction in less than 1000 sec instead of days. The chosen organic guests were 3-carboxy coumarin and, given their importance, a series of non-steroidal anti-inflammatory drugs with different pKa values and steric hindrance; namely ketoprofen, flurbiprofen, ibuprofen, indomethacin and tiaprofenic acid. The method has been applied to different classes of compounds to characterize the reaction in terms of speed, yield and also applicability. The characterization of the obtained nano-composites, carried out by crystallographic and microscopic techniques, revealed that the synthesis yield is comparable to that of standard methods, but with enormous time, solvent, and energy saving advantages. Moreover, the in situ diffraction experiments allowed to shed some light on the kinetics of the intercalation process with sub-second resolution and to determine the parameters affecting the reaction. Steric hindrance of the molecule proved to be the most relevant parameter to de-termine the applicability of this method. Finally we also show that our method can be easily up scaled.
2013
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11391/989186
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