Nickel oxalate micro-spheres with core-shell structure of solid core and radiate shell were synthesized by precipitation method in a mixed water solution, with oxalic acid and nickel acetate as raw materials, through ...Nickel oxalate micro-spheres with core-shell structure of solid core and radiate shell were synthesized by precipitation method in a mixed water solution, with oxalic acid and nickel acetate as raw materials, through dropping ammonium hydroxide to adjust the solution pH value to about 8.0. Nickel microspheres with core-shell structure of solid core and porous shell were prepared by decomposing of nickel oxalate microspheres precursor at about 340 ℃ in argon atmosphere. The analyses of infrared spectroscopy(IR)indicates that the composition of the powders is nickel oxalate. The analyses of atomic absorption spectrometry(AAS) and organic elemental analysis(OEA) indicate that the molar ratio of(C2O4)^2-/Ni^2+ is about 1.02, close to the theoretical value of 1.0. The results of the thermo-gravimetric and differential thermal gravity analyses(TG-DTG) indicate that the molar ratio of(C2O4)^2-/Ni^2+ is about 1.06, also close to the theoretical value of 1.0.The analysis of X-ray diffraction(XRD) indicates that the composition of black powders as-prepared is nickel,which has a face-centered cubic crystal structure with average crystal grain size about 16.87 nm. The images of scanning electron microscopy(SEM) indicate that the morphology of nickel oxalate microspheres is a coreshell structure with solid core and radiate shell. The diameter of nickel oxalate microspheres is about 3 μm, and the shell consists of a large number of thin nanorods. The images of SEM also indicate that the morphology of nickel microspheres is a core-shell structure with solid core and porous shell. The diameter of nickel microspheres is about 2 μm, and the shell consists of a large number of nickel grains, surface holes and through holes. The diameter of nickel grains is about 50-100 nm, and the diameter of holes is about 50-200 nm.展开更多
The effect of ethanedioic acid（Ed A） functionalization on Al2O3 supported Ni catalyst was studied on the hydrodeoxygenation（HDO）, isomerization, kinetics and Arrhenius parameters of octadec-9-enoic acid（OA） into...The effect of ethanedioic acid（Ed A） functionalization on Al2O3 supported Ni catalyst was studied on the hydrodeoxygenation（HDO）, isomerization, kinetics and Arrhenius parameters of octadec-9-enoic acid（OA） into biofuel in this report. This was achieved via synthesis of two catalysts; the first, nickel alumina catalyst（Ni/Al2O3） was via the incorporation of inorganic Ni precursor into Al2O3; the second was via the incorporation nickel oxalate（Ni Ox） prepared by functionalization of Ni with Ed A into Al2O3 to obtain organometallic Ni Ox/Al2O3 catalyst. Their characterization results showed that Ni species present in Ni/Al2O3 and Ni Ox/Al2O3 were 8.2% and 9.3%, respectively according to the energy dispersive X-ray result. Ni Ox/Al2O3 has comparably higher Ni content due to the Ed A functionalization which also increases its acidity and guarantees high Ni dispersion with weaker metal-support-interaction leading to highly reducible Ni as seen in the X-ray diffraction, X-ray photoelectron spectroscopy, TPR and Raman spectroscopy results. Their activities tested on the HDO of OA showed that Ni Ox/Al2O3 did not only display the best catalytic and reusability abilities, but it also possesses isomerization ability due to its increased acidity. The Ni Ox/Al2O3 also has the highest rate constants evaluated using pseudo-first-order kinetics,but the least activation energy of 176 k J/mol in the biofuel formation step compared to 244 k J/mol evaluated when using Ni/Al2O3. The result is promising for future feasibility studies toward commercialization of catalytic HDO of OA into useful biofuel using organometallic catalysts.展开更多
基金Funded by the National Natural Science Foundation of China(51002126)the Opening Project of Material Corrosion and Protection Key Laboratory of Sichuan Province(2017CL20)
文摘Nickel oxalate micro-spheres with core-shell structure of solid core and radiate shell were synthesized by precipitation method in a mixed water solution, with oxalic acid and nickel acetate as raw materials, through dropping ammonium hydroxide to adjust the solution pH value to about 8.0. Nickel microspheres with core-shell structure of solid core and porous shell were prepared by decomposing of nickel oxalate microspheres precursor at about 340 ℃ in argon atmosphere. The analyses of infrared spectroscopy(IR)indicates that the composition of the powders is nickel oxalate. The analyses of atomic absorption spectrometry(AAS) and organic elemental analysis(OEA) indicate that the molar ratio of(C2O4)^2-/Ni^2+ is about 1.02, close to the theoretical value of 1.0. The results of the thermo-gravimetric and differential thermal gravity analyses(TG-DTG) indicate that the molar ratio of(C2O4)^2-/Ni^2+ is about 1.06, also close to the theoretical value of 1.0.The analysis of X-ray diffraction(XRD) indicates that the composition of black powders as-prepared is nickel,which has a face-centered cubic crystal structure with average crystal grain size about 16.87 nm. The images of scanning electron microscopy(SEM) indicate that the morphology of nickel oxalate microspheres is a coreshell structure with solid core and radiate shell. The diameter of nickel oxalate microspheres is about 3 μm, and the shell consists of a large number of thin nanorods. The images of SEM also indicate that the morphology of nickel microspheres is a core-shell structure with solid core and porous shell. The diameter of nickel microspheres is about 2 μm, and the shell consists of a large number of nickel grains, surface holes and through holes. The diameter of nickel grains is about 50-100 nm, and the diameter of holes is about 50-200 nm.
基金financial support from Higher Impact Research-Ministry of Higher Education project no D000011-16001 of the Faculty of Engineering,University of Malaya,Malaysia and the Mitsubishi Corporation Education Trust Fund,University Teknologi PETRONAS,Malaysia
文摘The effect of ethanedioic acid（Ed A） functionalization on Al2O3 supported Ni catalyst was studied on the hydrodeoxygenation（HDO）, isomerization, kinetics and Arrhenius parameters of octadec-9-enoic acid（OA） into biofuel in this report. This was achieved via synthesis of two catalysts; the first, nickel alumina catalyst（Ni/Al2O3） was via the incorporation of inorganic Ni precursor into Al2O3; the second was via the incorporation nickel oxalate（Ni Ox） prepared by functionalization of Ni with Ed A into Al2O3 to obtain organometallic Ni Ox/Al2O3 catalyst. Their characterization results showed that Ni species present in Ni/Al2O3 and Ni Ox/Al2O3 were 8.2% and 9.3%, respectively according to the energy dispersive X-ray result. Ni Ox/Al2O3 has comparably higher Ni content due to the Ed A functionalization which also increases its acidity and guarantees high Ni dispersion with weaker metal-support-interaction leading to highly reducible Ni as seen in the X-ray diffraction, X-ray photoelectron spectroscopy, TPR and Raman spectroscopy results. Their activities tested on the HDO of OA showed that Ni Ox/Al2O3 did not only display the best catalytic and reusability abilities, but it also possesses isomerization ability due to its increased acidity. The Ni Ox/Al2O3 also has the highest rate constants evaluated using pseudo-first-order kinetics,but the least activation energy of 176 k J/mol in the biofuel formation step compared to 244 k J/mol evaluated when using Ni/Al2O3. The result is promising for future feasibility studies toward commercialization of catalytic HDO of OA into useful biofuel using organometallic catalysts.
