Name: chemical precipitation method for the synthesis of nb2o5 modified bulk nickel catalysts with high specific surface area
Uploaded: 2018-02-19T15:00:00
Description: Watch this Scientific Journal Video about Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area at JoVE.com

We gratefully acknowledge the financial support provided by National Key Research &#38; Development Program of the Ministry of Science and Technology of China (2016YFB0600305), National Natural Science Foundation of China (Nos. 21573031 and 21373038), Program for Excellent Talents in Dalian City (2016RD09) and Technological and Higher Education Institute of Hong Kong (THEi SG1617105 and THEi SG1617127).

Caution: For the proper handling methods, properties and toxicities of the chemicals described in this paper, refer to the relevant material safety data sheets (MSDS). Some of the chemicals used are toxic and carcinogenic and special cares must be taken. Nanomaterials may potentially pose safety hazards and health effects. Inhalation and skin contact should be avoided. Safety precaution must be exercised, such as performing the catalyst synthesis in the fume hood and catalyst performance evaluation with ...

<ol>
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One of the common methods to prepare the nickel-doped bulk niobium oxide nanoparticles is rotary evaporation method.9 By employing various pressure and temperature conditions during the process of rotary evaporation, the precipitation of Ni-Nb-O particles commerce with the slow removal of the solvent. In contrast to the rotary evaporation method, the chemical precipitation method reported in this study has received increasing attention to prepare the nanoparticles as this do not require the remova...

The preparation of nanocomposites has received increasing attention due to their crucial application in various field. To prepare Ni-Nb-O mixed oxide nanoparticles,1,2,3,4,5,6 different methods have been developed such as dry mixing method,7,8 evaporation method,9,10,11,12,13 sol gel method,14 thermal decomposition method,15 and auto-combustion.16 In a typical evaporation method9, aqueous solutions containing the appropriate amount of metal precursors, nickel nitrate hexahydrate and ammonium niobium oxalate were heated at 70 &#176;C. After the removal of solvent and further drying and calcination, the mixed oxide was obtained. These oxide catalysts exhibit excellent catalytic activity and selectivity towards the oxidative dehydrogenation (ODH) of ethane, which is related to the electronic and structural rearrangement induced by the incorporation of niobium cations in the NiO lattice.11 The insertion of Nb drastically decreases the electrophilic oxygen species, which is responsible for the oxidation reactions of ethane12. As a result, extensions of this method have been done on the preparation of different types of mixed Ni-Me-O oxides, where Me = Li, Mg, Al, Ga, Ti and Ta.13 It is found that the variation of metal dopants could alter the unselective and electrophilic oxygen radicals of NiO, thus systematically tune the ODH activity and selectivity towards ethane. However, generally the surface area of these oxides is relatively small (&#60; 100 m2/g), due to the extended phase segregation and formation of large Nb2O5 crystallites, and thus hampered their uses in other catalytic applications.
Dry mixing method, also known as the solid-state grinding method, is another commonly used method to prepare the mixed-oxide catalysts. Since the catalytic materials are obtained in a solvent-free way, this method provides a promising green and sustainable alternative to the preparation of mixed-oxide. The highest surface area obtained by this method is 172 m2/g for Ni80Nb20 at calcination temperature of 250 &#176;C.8 However, this solid-state method is not reliable as reactants are not well mixed on the atomic scale. Therefore, for better control of chemical homogeneity and specific particle size distribution and morphology, other suitable methods to prepare Ni-Nb-O mixed oxide nanoparticles are still being sought.7
Among various strategies in the development of nanoparticles, chemical precipitation serves as one of the promising methods to develop the nanocatalysts, since it allows the complete precipitation of the metal ions. Also, nanoparticles of higher surface areas are commonly prepared by using this method. To improve the catalytic properties of Ni-Nb-O nanoparticles, we herein report the protocol for the synthesis of a series of Ni-Nb-O mixed oxide catalysts with high surface area by chemical precipitation method. We demonstrated that the Nb:Ni molar ratio is a crucial factor in determining the catalytic activity of the oxides towards the hydrodeoxygenation of lignin-derived organic compounds. With high Nb:Ni ratio above 0.087, inactive NiNb2O6 species were formed. Ni0.92Nb0.08O, which had the largest surface area (173 m2/g), exhibits fold-like nanosheets structures and showed the best activity and selectivity towards the hydrodeoxygenation of anisole to cyclohexane.

<table>
	<tbody>
		<tr>
			<td>Niobium(V) oxalate hydrate, 98%</td>
			<td>Alfa</td>
			<td>L04481902</td>
			<td></td>
		</tr>
		<tr>
			<td>Nickel nitrate hexahydrate, 99%</td>
			<td>Aladdin</td>
			<td>N108891</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium hydroxide, 98%</td>
			<td>Aladdin</td>
			<td>S111501</td>
			<td></td>
		</tr>
		<tr>
			<td>Ammonium hydroxide, 23-25%</td>
			<td>Aladdin</td>
			<td>A112077</td>
			<td></td>
		</tr>
		<tr>
			<td>Anisole, 99%</td>
			<td>Sinopharm</td>
			<td>81001728</td>
			<td></td>
		</tr>
		<tr>
			<td>Diphenyl ether, 98%</td>
			<td>Aladdin</td>
			<td>D110644</td>
			<td></td>
		</tr>
		<tr>
			<td>Phenol, 98%</td>
			<td>Sinopharm</td>
			<td>100153008</td>
			<td></td>
		</tr>
		<tr>
			<td>2-Methoxyphenol, 98%</td>
			<td>Sinopharm</td>
			<td>30114526</td>
			<td></td>
		</tr>
		<tr>
			<td>Vanillin, 99.5%</td>
			<td>Sinopharm</td>
			<td>69024316</td>
			<td></td>
		</tr>
		<tr>
			<td>Potassium hydroxide, AR</td>
			<td>Aladdin</td>
			<td>P112284</td>
			<td></td>
		</tr>
		<tr>
			<td>N,N-Dimethylformamide, 99.5%</td>
			<td>Sinopharm</td>
			<td>40016462</td>
			<td></td>
		</tr>
		<tr>
			<td>2-Bromoacetophenone,98%</td>
			<td>Aladdin</td>
			<td>B103328</td>
			<td></td>
		</tr>
		<tr>
			<td>Diethyl ether,99.5%</td>
			<td>Sinopharm</td>
			<td>10009318</td>
			<td></td>
		</tr>
		<tr>
			<td>Decane,98%</td>
			<td>Aladdin</td>
			<td>D105231</td>
			<td></td>
		</tr>
		<tr>
			<td>Dodecane,99%</td>
			<td>Aladdin</td>
			<td>D119697</td>
			<td></td>
		</tr>
		<tr>
			<td>Niobic acid</td>
			<td>CBMM</td>
			<td>1313968</td>
			<td></td>
		</tr>
		<tr>
			<td>Heating and Drying Oven</td>
			<td></td>
			<td></td>
			<td>DHG Series (shanghai jinghong laboratory instrument co. ltd)</td>
		</tr>
		<tr>
			<td>Autoclave Reactor</td>
			<td></td>
			<td></td>
			<td>CJF-0.05&#8212;0.1L (Dalian Tongda Equipment Technology Development Co., Ltd)</td>
		</tr>
		<tr>
			<td>Tube&#160;furnace</td>
			<td></td>
			<td></td>
			<td>SK2-1-10/12 (Luoyang Huaxulier Electric Stove Co., Ltd)</td>
		</tr>
		<tr>
			<td>Heating magnetic stirrer</td>
			<td></td>
			<td></td>
			<td>DF-101 (Yu Hua Instrument Co. Ltd.)</td>
		</tr>
		<tr>
			<td>Rotary evaporator</td>
			<td></td>
			<td></td>
			<td>RE-3000A (Shanghai Yarong Biochemical Instrument Factory)</td>
		</tr>
		<tr>
			<td>Synthetic air</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Hydrogen gas</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Argon gas</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

chemical precipitation method for the synthesis of nb2o5 modified bulk nickel catalysts with high specific surface area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

X-ray diffraction (XRD) patterns (Figure 1 and Figure 2), BET surface areas, temperature-programmed reduction of hydrogen with hydrogen (H2-TPR), scanning electron microscopy (SEM) equipped with an energy-dispersive X-ray (EDX) analyzer, X-ray photoelectron spectroscopy (XPS) were collected for the nanoparticles NiO, Ni-Nb-O and Nb2O5 oxides17 (Figure 3...

Watch this Scientific Journal Video about Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area at JoVE.com

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Research

JoVE Journal

Chemistry

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

A Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

Synthesis and Characterization of 1,2-Dithiolane Modified Self-Assembling Peptides

This report focuses on the synthesis of an N-terminus 1,2-dithiolane modified self-assembling peptide and the characterization of the resulting ...

Synthesis and Bioconjugation of Thiol-Reactive Reagents for the Creation of Site-Selectively Modified Immunoconjugates

Maleimide-bearing bifunctional probes have been employed for decades for the site-selective modification of thiols in biomolecules, especially antibodies. ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...