Method for preparing nickel-tungsten bimetallic carbide catalyst by organic-inorganic hybrid route and application of nickel-tungsten bimetallic carbide catalyst

A bimetallic carbide and catalyst technology, which is applied in the direction of catalyst activation/preparation, hydrocarbon production from oxygen-containing organic compounds, physical/chemical process catalysts, etc., can solve the problem of reducing catalyst active sites, limiting carbide materials, and polymer carbon Pollution and other issues, to achieve the effect of optimistic industrial application prospects, simple operation, and energy-saving product particles

Active Publication Date: 2017-12-26
DALIAN UNIV OF TECH
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  • Abstract
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  • Application Information

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Problems solved by technology

And it is difficult to completely convert, because the reaction only occurs at the gas-solid interface
Meanwhile, the pyrolysis of excess carbon-containing gas easily leads to polymer carbon contamination on the surface of bimetallic carbide particles, seriously reducing the active sites of the catalyst.
In addition, stringent and complex synthesis conditions, such as precise control of the temperature increase rate (generally not greater than 1 °C / min) and gas composition and flow rate, severely limit the large-scale fabrication of carbide materials.
[0004] At present, there are relatively few reports on the preparation of nickel-tungsten bimetallic carbides (Xiao T C, Wang H T, York A P E, et al.Preparation of nickel-tungsten bimetallic carbide catalysts[J].J Catal,2002,209(2) :318-330 and Al-Megren H A, Gonzalez-Cortes S L, Xiao T, et al.A comparative study of the catalytic performance of Co-Mo and.Co(Ni)-Wcarbide catalysts in the hydrogenenitrogenation(HDN)reaction of pyridine[ J].Applied Catalysis a-General,2007,329:36-45.), and the reported nickel-tungsten double metal carbides often have phase separation

Method used

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  • Method for preparing nickel-tungsten bimetallic carbide catalyst by organic-inorganic hybrid route and application of nickel-tungsten bimetallic carbide catalyst
  • Method for preparing nickel-tungsten bimetallic carbide catalyst by organic-inorganic hybrid route and application of nickel-tungsten bimetallic carbide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 0.43g melamine (C 3 N 3 (NH 2 ) 3 ) and 1g ammonium metatungstate ((NH 4 ) 6 h 2 W 12 o 40 ·nH 2 O) Add 150 mL of deionized water, and heat to 70° C. under magnetic stirring. After the melamine and ammonium metatungstate are completely dissolved, raise the temperature to 90°C, slowly form a white milky liquid, keep stirring at 90°C for 12 hours, then collect the white precipitate from the suspension by centrifugation, wash with deionized water and ethanol After several times, dry in an oven at 80°C for 24 hours to obtain ammonium metatungstate-melamine hybrid.

[0025] 0.75g Ni(NO 3 ) 2 ·6H 2 O was dissolved in 1.6 mL of water, then added dropwise to a tube containing 1 g of the hybrid, sonicated for 30 min, and then dried at 90 °C for 24 h. An organic-inorganic hybrid having an atomic ratio of W:Ni=1 is thus obtained.

[0026] The ammonium metatungstate-melamine hybrid (1 g) containing nickel nitrate was placed in a quartz boat in a quartz tube reactor an...

Embodiment 2

[0028] 4.3g melamine (C 3 N 3 (NH 2 ) 3 ) and 20g sodium metatungstate ((NH 4 ) 6 h 2 W 12 o 40 ·nH 2 O) Add 3050mL of deionized water and heat to 70°C under magnetic stirring. After the melamine and ammonium metatungstate are completely dissolved, raise the temperature to 80°C, slowly form a white milky liquid, keep stirring at 80°C for 24 hours, then collect the white precipitate from the suspension by centrifugation, wash with deionized water and ethanol After several times, dry in an oven at 80°C for 24 hours to obtain ammonium metatungstate-melamine hybrid.

[0029] 0.375g Ni(NO 3 ) 2 ·6H 2 O was dissolved in 1.6 mL of water, then added dropwise to a tube containing 1 g of the hybrid, sonicated for 50 min, and then dried at 90 °C for 24 h. An organic-inorganic hybrid having an atomic ratio of W:Ni=2 is thus obtained.

[0030] The ammonium metatungstate-melamine hybrid (1 g) containing nickel nitrate was placed in a quartz boat in a quartz tube reactor and py...

Embodiment 3

[0032] 1g melamine (C 3 N 3 (NH 2 ) 3 ) and 0.2g ammonium metatungstate ((NH 4 ) 6 h 2 W 12 o 40 ·nH 2 O) Add 150mL of deionized water and heat to 60°C under magnetic stirring. After the melamine and ammonium metatungstate are completely dissolved, raise the temperature to 95°C, slowly form a white milky liquid, keep stirring at 95°C for 6 hours, then collect the white precipitate from the suspension by centrifugation, wash with deionized water and ethanol After several times, dry in an oven at 80°C for 24 hours to obtain ammonium metatungstate-melamine hybrid.

[0033] 0.1875g Ni(NO 3 ) 2 ·6H 2 O was dissolved in 1.6 mL of water, then added dropwise to a tube containing 1 g of the hybrid, sonicated for 90 min, and then dried at 90 °C for 24 h. An organic-inorganic hybrid having an atomic ratio of W:Ni=4 is thus obtained.

[0034] The ammonium metatungstate-melamine hybrid (1 g) containing nickel nitrate was placed in a quartz boat in a quartz tube reactor and py...

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Abstract

The invention discloses a method for preparing a nickel-tungsten bimetallic carbide catalyst by an organic-inorganic hybrid route and application of the nickel-tungsten bimetallic carbide catalyst, and belongs to the technical field of material preparation and application. The method is characterized in that pure phase Ni6W6C and W2C and Ni6W6C composite materials with different Ni contents are synthesized by the organic-inorganic hybrid route and both exhibit a nano-particle stacking and aggregation form with a length of about 0.3-4 mu m and a diameter of about 300-900 nm. The BET specific surface area of the nickel-tungsten bimetallic carbide ranges from 17.6 m<2> / g to 15.7 m<2> / g. Compared with the traditional arc melting method and temperature programmed reduction method, the method provided by the invention has the advantages of low temperature, simple operation, energy saving, small product particles and less surface carbon pollution. The industrial application prospect is optimistic, the prepared bimetallic carbide catalyst can be applied to hydrogenation, hydrogenolysis, dehydrogenation, deoxygenation, isomerization, methane syngas, water-gas shift, hydrogen evolution reaction and catalyst support and the like.

Description

technical field [0001] The invention belongs to the field of material preparation technology and application, and relates to an organic-inorganic hybrid route for preparing a nickel-tungsten double metal carbide catalyst and its application. Background technique [0002] Nickel-tungsten bimetallic carbide catalysts have a wide range of applications and can be used for hydrogenation, hydrogenolysis, dehydrogenation, deoxygenation, isomerization, methane synthesis gas, water gas shift, hydrogen evolution reaction and catalyst support. [0003] At present, there have been many methods for the synthesis of nickel-tungsten bimetallic carbides. The earliest attempt was the arc melting method, which required high energy consumption due to the high temperature and long annealing time required, and the product usually had a low surface area, which limited its application in catalysis. Another common method is the temperature-programmed reduction method, through which hydrocarbon gas...

Claims

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Application Information

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IPC IPC(8): B01J27/22B01J37/00C07C1/20C07C13/18C07C15/073
CPCB01J27/22B01J37/00C07C1/20C07C13/18C07C15/073Y02P20/10
Inventor 梁长海刘荣李闯陈晓贞
Owner DALIAN UNIV OF TECH
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