By electron paramagnetic resonance (EPR), coupled to elemental and thermogravimetric analysis and diffuse reflectance spectroscopy (DRS), we investigated the unusual quasi-complete reduction of Cu2+ species in Cu-ZSM- 5 zeolites (Si/Al = 80 and 25) at different copper loadings induced by high-temperature vacuum treatments. It has been found that at high temperatures (673-773 K) in vacuum a quasi-complete reduction of Cu2+ unexpectedly occurred in all the "as-prepared Cu-ZSM-5 samples. Evidence is given that such extensive reduction of Cu2+ species is caused by carbonaceous deposits. In order to completely remove any residual carbonaceous species, the "as-prepared" Cu-ZSM-5 materials must be heated in air (or O2) at high temperature (673-773 K) for prolonged time. Differently, some carbon residue, as in particular originated from the organic template used in the zeolite synthesis, can be left within the channels of the ZSM-5 structure. We show also that such a carbon residue, even when escapes the detection accuracy of elemental analysis, can be checked by a careful EPR characterization. KEYWORDS: Cu-ZSM-5 zeolites, reduction of Cu2+ species by carbonaceous deposits, EPR evidence of organic template residue, DRS characterization, EPR characterization
UNUSUAL COMPLETE REDUCTION OF Cu2+ SPECIES IN Cu-ZSM- 5 ZEOLITES UNDER VACUUM TREATMENT AT HIGH TEMPERATURE
FIERRO G;FERRARIS G;
2012
Abstract
By electron paramagnetic resonance (EPR), coupled to elemental and thermogravimetric analysis and diffuse reflectance spectroscopy (DRS), we investigated the unusual quasi-complete reduction of Cu2+ species in Cu-ZSM- 5 zeolites (Si/Al = 80 and 25) at different copper loadings induced by high-temperature vacuum treatments. It has been found that at high temperatures (673-773 K) in vacuum a quasi-complete reduction of Cu2+ unexpectedly occurred in all the "as-prepared Cu-ZSM-5 samples. Evidence is given that such extensive reduction of Cu2+ species is caused by carbonaceous deposits. In order to completely remove any residual carbonaceous species, the "as-prepared" Cu-ZSM-5 materials must be heated in air (or O2) at high temperature (673-773 K) for prolonged time. Differently, some carbon residue, as in particular originated from the organic template used in the zeolite synthesis, can be left within the channels of the ZSM-5 structure. We show also that such a carbon residue, even when escapes the detection accuracy of elemental analysis, can be checked by a careful EPR characterization. KEYWORDS: Cu-ZSM-5 zeolites, reduction of Cu2+ species by carbonaceous deposits, EPR evidence of organic template residue, DRS characterization, EPR characterizationI documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
