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Preparation method of transition metal carbide catalyst and its catalytic performance

A technology of transition metals and carbides, which is applied in the field of preparation of transition metal single-component and double-component carbides, can solve the problem of high reaction temperature, achieve high activity, good activity and selectivity, and simple and easy preparation process Effect

Inactive Publication Date: 2004-10-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Ledoux et al. used the carbothermal reduction method to react metal compound vapor with carbon materials (M.J.Ledoux, et al., U.S. Pat. No. 4914070, 1990), and prepared carbides with high specific surfaces, but the reaction temperature was higher (1000 °C above)

Method used

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  • Preparation method of transition metal carbide catalyst and its catalytic performance
  • Preparation method of transition metal carbide catalyst and its catalytic performance
  • Preparation method of transition metal carbide catalyst and its catalytic performance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation of embodiment 1 molybdenum carbide precursor

[0023] Dissolve molybdate (preferably ammonium molybdate) or ammonium phosphomolybdate in water or ammonia water to form an impregnation solution, add activated carbon carrier and impregnate for 2 hours. Activated carbon surface area is 1000m 2 / g. Evaporate the solution under stirring, then bake at 100°C for 10 hours, and treat in an inert atmosphere or vacuum at 200°C to obtain a molybdenum carbide precursor. Molybdenum carbide precursors with different loads can be prepared by changing the amount of impregnating solution added.

Embodiment 2

[0024] The preparation of embodiment 2 nickel carbide precursor

[0025] Molybdate (preferably adopting ammonium molybdate) and nickel salt (such as nickel nitrate, nickel oxalate, etc.) are dissolved in water or ammonia water to form a uniform solution, then add the activated carbon carrier described in Example 1 and impregnate for 5 hours, stir Evaporate the solution, then bake at 110°C for 15 hours, and treat in an inert atmosphere or vacuum at 300°C to obtain the precursor of nickel molybdenum carbide.

[0026] The nickel-molybdenum carbide precursor can also be impregnated in steps, that is, the molybdate is impregnated first and then the nickel salt is impregnated, or the nickel salt is impregnated first and then the molybdate is impregnated. After each step of impregnation, the solution needs to be evaporated under stirring, then baked at 100-120°C for 10-24 hours, and treated in an inert atmosphere or vacuum at 200-400°C to finally obtain the precursor of nickel molybd...

Embodiment 3

[0028] The preparation of embodiment 3 cobalt molybdenum carbide precursor

[0029] Molybdate (preferably adopting ammonium molybdate) and cobalt salt (as cobalt nitrate, cobalt oxalate etc.) are dissolved in water or ammoniacal liquor to form homogeneous solution, then add the gac carrier described in embodiment 1 and impregnate 10 hours, stir Evaporate the solution, then bake at 120°C for 24 hours, and treat in an inert atmosphere or vacuum at 400°C to obtain the cobalt-molybdenum carbide precursor.

[0030] The nickel-molybdenum carbide precursor can also be impregnated in steps, that is, the molybdate is impregnated first and then the cobalt salt is impregnated, or the cobalt salt is impregnated first and then the molybdate is impregnated. After each step of impregnation, the solution needs to be evaporated under stirring, then baked at 100-120°C for 10-24 hours, and treated in an inert atmosphere or vacuum at 200-400°C to finally obtain a cobalt-molybdenum carbide precurs...

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Abstract

The present invention discloses a preparation method of catalyst for preparing transition metal carbide, its precursor is formed from carbon material and transition metal compound. Said invention adopts the impregnation or mechanical mixing method to load the transmition metal on the carbon material, and the weight percentage of the transition metal compound loaded quantity is in the range of 1-200%, and the obtained sample can be heated to 500-1000 deg.C in heating rate of 1-20 deg.C / min under the atmosphere of hydrogen gas, then thermostatic reduced for 0.1-10 hr, and reduced to room temp. and passivated by using 1% of oxygen gas under the atmosphere of hydrogen gas or reduced to room temp. under the inert-atmosphere so as to obtain the correspondent transion metal carbide or transition metal carbide loaded on the carbon material.

Description

technical field [0001] The invention relates to a method for preparing transition metal single-unit and double-unit carbides. Specifically, the conversion of transition metal compounds into transition metal carbides by carbothermal hydrogen reduction method and the application of the prepared transition metal carbides as catalysts. Background technique [0002] Transition metal carbides are a class of mesenchymal compounds produced by embedding carbon atoms into transition metal lattices, which have the properties of covalent solids, ionic crystals, and transition metals. Since the discovery of transition metal carbides with noble metal-like properties in the 1970s, transition metal carbides have received great attention in the field of catalysis. Transition metal carbides have unique reactivity to reactions such as ammonia synthesis and decomposition, hydrofining, selective hydrogenation, and isomerization. The temperature-programmed carbonization method developed by Boud...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/22C01B31/30
Inventor 梁长海李灿应品良孙福侠
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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