Ethanol,
especially that produced from biomass, is considered as
a renewable and carbon-neutral candidate to produce hydrogen. Performances
of NiFe–MgAl bifunctional catalysts, in terms of activity,
stability, and regenerability, in chemical looping reforming (CLR)
of ethanol were studied. The NiFe–MgAl bifunctional catalysts
were prepared from hydrotalcite-like compounds by the co-precipitation
method. Various characterization techniques, that is, X-ray diffraction,
inductively coupled plasma, nitrogen adsorption/desorption, H2-temperature-programmed reduction, and transmission electron
microscopy, were used to determine properties of fresh and spent catalysts.
In addition, O2 temperature-programmed oxidation, scanning
electron microscopy, and Raman analyses were used for observation
of coke formation on the spent catalysts. Meanwhile, in situ diffuse reflectance infrared Fourier transform spectroscopy can
verify the evolution of the catalyst during the reactions. It was
observed that the NiFe–MgAl catalyst showed higher catalytic
activity and stability than the monometallic Fe–MgAl and Ni–MgAl
catalysts. More specifically, the NiFe–MgAl catalyst provided
the highest H2 concentration up to 80% at a low reaction
temperature of 500 °C. This high performance was ascribed to
the formation of Ni–Fe alloy particles. The combination of
pulse experiments and X-ray photoelectron spectroscopy analysis elucidated
that the iron particle at the surface was in the form of FeO that
can oxidize the carbon deposits, resulting in the suppression of coke
formation. In addition, the NiFe–MgAl catalyst can maintain
high hydrogen selectivity for 10 repeated cycles.