Ni3P shows extremely high activity and stability in phenol hydrodeoxygenation both in the aqueous phase and in the organic phase.

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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.

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Organic aerogels and related carbon aerogels were prepared from the NaOH-catalyzed polycondensation of resorcinol-furfural (RF) and supercritical drying in ethanol. The effect of the preparation conditions, including the RF concentration, molar ratio of resorcinol (R) to NaOH, and molar ratio of R to furfural, on the gelation time and bulk density was studied. The chemical structure of the organic aerogel was revealed by IR spectroscopy. The pyrolysis process of the organic aerogel was investigated by thermogravimetric analysis. According to characterizations of transmission electron microscopy and nitrogen adsorption, the organic and carbon aerogels we obtained had a threedimensional network that consisted of around 30-nm particles, which defined numerous mesopores of less than 30 nm. As a result, the aerogels had high Brunauer-EmmettTeller surface areas (698 -753 m 2 /g) and large mesopore volumes (1.09 -1.64 cm 3 /g). X-ray diffraction characterization indicated that the carbon aerogel was more crystalline than activated carbon but less activated than graphite.

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Unsupported Ni 3 P-CePO 4 catalysts were prepared by coprecipitation, followed by drying, calcination, and temperature-programmed reduction. The prepared catalysts were characterized by XRD, N 2 adsorption−desorption, TEM, STEM-EDS elemental mapping, XPS, NH 3 -TPD, FT-IR of adsorbed pyridine, and H 2 -TPR. Their catalytic performances in hydrodeoxygenation (HDO) were investigated using an aqueous solution of phenol (5.0 wt %) as the feed. CePO 4 was generated in coprecipitation and stable in the subsequent drying, calcination, and temperature-programmed reduction (final temperature 500 °C). It is shown that the addition of CePO 4 resulted in enhanced HDO activity, and a maximum activity appeared at a Ce/Ni ratio of 0.3. The presence of CePO 4 improved the dispersion of Ni 3 P significantly, leading to enhanced hydrogenation activity. CePO 4 served as the major dehydration sites as well because of its surface acidity (mainly Lewis acid). In addition, the kinetics of the aqueous phase HDO of phenol and cyclohexanol catalyzed by Ni 3 P and by Ni 3 P-CePO 4 with Ce/Ni ratio of 0.3 were investigated.

Reaction of a semirigid ligand with two octahedral metal ions with restricted coordination symmetry afforded metalated container complexes showing trigonal or tetragonal outer shapes and inner cavities.