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

3 Cites 7 Cited by

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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] A...

Method used

[0026] The ammonium metatungstate-melamine hybrid (1g) containing nickel nitrate is placed in the quartz boat in the quartz tube reactor, and pyrolysis is carried out under an inert atmosphere. After replacing the air with argon at room temperature for 3 hours, the temperature was linearly increased to 750°C at a rate of 1°C/min under an atmosphere of argon (7...

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.

Application Domain

Chemical industryCatalyst activation/preparation +1

Technology Topic

DeoxygenationTungsten +16

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Examples

Experimental program(7)

Example Embodiment

[0023] Example 1

[0024] 0.43g of 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, the temperature is increased to 90°C, and a white milky liquid is slowly formed. Keep stirring at 90°C for 12 hours, and then collect the white precipitate from the suspension by centrifugation, and wash with deionized water and ethanol After several times, it was dried in an oven at 80° C. for 24 hours to obtain an ammonium metatungstate-melamine hybrid.

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

[0026] The ammonium metatungstate-melamine hybrid (1 g) containing nickel nitrate was placed in a quartz boat in a quartz tube reactor, and pyrolyzed under an inert atmosphere. After replacing the air with argon at room temperature for 3 hours, the temperature was linearly increased to 750°C at a rate of 1°C/min under an argon atmosphere (70mL/min) and maintained for 4 hours. The obtained product was slowly cooled to room temperature. , Shut off the gas to allow the air to slowly diffuse back into the tube to passivate the carbide surface, thereby avoiding violent oxidation reaction and bulk oxidation. Get pure phase Ni 6 W 6 C, XRD characterization results are as figure 1 Shown.

Example Embodiment

[0027] Example 2

[0028] Put 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 3050 mL of deionized water and heat to 70°C under magnetic stirring. After the melamine and ammonium metatungstate are completely dissolved, the temperature is increased to 80°C, and a white milky liquid is slowly formed. Keep the temperature at 80°C and keep stirring for 24 hours, and then collect the white precipitate from the suspension by centrifugation, and wash it with deionized water and ethanol After several times, it was dried in an oven at 80° C. for 24 hours to obtain an 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 hybrid, treated with ultrasound for 50 minutes, and then dried at 90°C for 24 hours. Thus, an organic-inorganic hybrid containing an atomic ratio W:Ni=2 is obtained.

[0030] The ammonium metatungstate-melamine hybrid (1 g) containing nickel nitrate was placed in a quartz boat in a quartz tube reactor, and pyrolyzed under an inert atmosphere. After replacing the air with argon at room temperature for 3 hours, the temperature was linearly increased to 850°C at a rate of 5°C/min under an argon (70mL/min) atmosphere and maintained for 4 hours. The obtained product was slowly cooled to room temperature. , Shut off the gas to allow the air to slowly diffuse back into the tube to passivate the carbide surface, thereby avoiding violent oxidation reaction and bulk oxidation. Get Ni 6 W 6 C and W 2 A mixture of C, where the atomic ratio W: Ni = 2, the XRD characterization results are as follows figure 2 Shown.

Example Embodiment

[0031] Example 3

[0032] Put 1g of 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 150 mL of deionized water and heat to 60°C under magnetic stirring. After the melamine and ammonium metatungstate are completely dissolved, the temperature is raised to 95°C, and a white milky liquid is slowly formed, kept at 95°C and kept stirring for 6 hours, and then the white precipitate is collected from the suspension by centrifugation, and washed with deionized water and ethanol After several times, it was dried in an oven at 80° C. for 24 hours to obtain an ammonium metatungstate-melamine hybrid.

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

[0034] The ammonium metatungstate-melamine hybrid (1 g) containing nickel nitrate was placed in a quartz boat in a quartz tube reactor, and pyrolyzed under an inert atmosphere. After replacing the air with argon at room temperature for 3 hours, the temperature was linearly increased to 650°C at a rate of 15°C/min under an argon (70mL/min) atmosphere and maintained for 4 hours. The obtained product was slowly cooled to room temperature. , Shut off the gas to allow the air to slowly diffuse back into the tube to passivate the carbide surface, thereby avoiding violent oxidation reaction and bulk oxidation. Get Ni 6 W 6 C and W 2 A mixture of C, where the atomic ratio W: Ni = 4, XRD characterization results are as follows figure 1 Shown.

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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

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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