A series of Ni3P-CePO4(x) catalysts were prepared by H2 temperature-programmed
reduction and utilized to catalyze the transfer hydrogenation (CTH)
of levulinic acid (LA) to γ-valerolactone (GVL). The characterization
of the synthesized catalysts was carried out by means of XRD, N2-adsorption/desorption, NH3-TPD, CO2-TPD, TEM, EDS elemental mapping, ICP, XPS, and TG/DSC. The effects
of Ce/Ni molar ratio, reaction temperature, reaction time, and hydrogen
donor on the CTH performance were studied. The yield of GVL was 89.9%
at an LA conversion of 99.9% at 180 °C for 2 h over the Ni3P-CePO4(0.1) catalyst using 2-propanol as the solvent.
The NH3-TPD and CO2-TPD measurements and poisoning
experiments verified that acidic/basic sites played a synergic role
in the process. A slight decrease in LA conversion and GVL yield was
observed after four consecutive cycles. The characterization of the
fresh and spent catalysts indicated that the minor deactivation was
due to the deposition of insoluble organics or polymers rather than
the changes of the crystal phase or acidic/basic properties, or the
leaching of the active sites.