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Synthesis method of nano-molybdenum carbide

A synthesis method and technology of molybdenum carbide, applied in the direction of carbides, tungsten/molybdenum carbides, etc., can solve the problems of complex precursor preparation, large product particles, and insufficient reaction, and achieve excellent catalytic performance, small particles, and process The effect of low conditional cost

Inactive Publication Date: 2014-07-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(3) Solvothermal reduction method, which is to use substances with strong reducing power (such as KBH 4 ) to reduce molybdenum oxide to molybdenum carbide, the method is simple and easy to control, the temperature is low, but the product is impure
(4) Metal precursor pyrolysis method, which is obtained by pyrolysis of a mixture of metal organic compounds and ammonium molybdate and hexamethylenetetramine. The product is relatively pure, but the preparation of the precursor is complicated, and the obtained particles are relatively large
In addition, there are reports of CVD, hydrothermal method, ultrasonic method, microwave method, etc., but these methods also have problems such as small yield, insufficient reaction, large product particles, and impure products.
The above methods are limited by their own shortcomings and have relatively large deficiencies in practical applications, especially in the mass production of catalysts.

Method used

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  • Synthesis method of nano-molybdenum carbide
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  • Synthesis method of nano-molybdenum carbide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) 0.1g of molybdenum trioxide was dissolved in 10mL of hydrogen peroxide with a mass fraction of 30wt%, placed in a water bath at 60°C and stirred for 2 hours;

[0029] (2) Dissolve 10g of glucose in 100mL of water;

[0030] (3) After mixing the two solutions in (1) and (2), place them in a water bath at 40°C and stir for 12 hours;

[0031] (4) The solution obtained in (3) was put into a 150mL autoclave, and hydrothermally treated at 180° C. for 6 hours to obtain a black product;

[0032] (5) After cooling the black product obtained in (4), wash it three times with deionized water, filter it, place it in an oven and dry it at 80°C for 24 hours until dry;

[0033] (6) Roast the product obtained in (5) at 700°C for 12 hours under an argon atmosphere of 30mL / min / gcat, and replace it with 2.0vol.%O after the temperature drops to 30°C 2 / Ar passivation gas, passivation treatment 12h, flow rate 5mL / min / gcat. The obtained sample was designated as MoC-1. Its phase paramet...

Embodiment 2

[0035] (1) 2g of ammonium molybdate was dissolved in 20mL of hydrogen peroxide with a mass fraction of 30wt%, placed in a water bath at 50°C and stirred for 2 hours;

[0036] (2) Dissolve 25g of sucrose in 100mL of water;

[0037] (3) After mixing the two solutions in (1) and (2), place them in a water bath at 40°C and stir for 12 hours;

[0038] (4) The solution obtained in (3) was put into a 150mL autoclave, and hydrothermally treated at 170° C. for 6 hours to obtain a black product;

[0039] (5) After cooling the black product obtained in (4), wash it three times with deionized water, filter it, place it in an oven and dry it at 80°C for 24 hours until dry;

[0040] (6) Roast the product obtained in (5) at 700°C for 12 hours under an argon atmosphere of 30mL / min / gcat, and replace it with 2.0vol.%O after the temperature drops to 30°C 2 / Ar passivation gas, passivation treatment 12h, flow rate 10mL / min / gcat. The resulting sample was designated MoC-2. Its phase parameters ...

Embodiment 3

[0042] (1) 2g of sodium molybdate was dissolved in 20mL of hydrogen peroxide with a mass fraction of 30wt%, placed in a water bath at 70°C and stirred for 2 hours;

[0043] (2) Dissolve 30g of maltose in 100mL of water;

[0044] (3) After mixing the two solutions in (1) and (2), place them in a water bath at 40°C and stir for 12 hours;

[0045] (4) The solution obtained in (3) was put into a 150mL autoclave, and hydrothermally treated at 190° C. for 6 hours to obtain a black product;

[0046](5) After cooling the black product obtained in (4), wash it three times with deionized water, filter it, place it in an oven and dry it at 80°C for 24 hours until dry;

[0047] (6) Roast the product obtained in (5) at 700°C for 12 hours under an argon atmosphere of 30mL / min / gcat, and replace it with 2.0vol.%O after the temperature drops to 30°C 2 / Ar passivation gas, passivation treatment for 12 hours, the flow rate is 15mL / min / gcat. The resulting sample was designated as MoC-3. Its p...

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Abstract

The invention relates to a synthesis method of nano-molybdenum carbide. The synthesis method comprises the following steps: dissolving a molybdenum precursor in hydrogen peroxide, dissolving carbohydrates in water, mixing the molybdenum precursor with the carbohydrates, stirring, loading a mixed solution into a hydrothermal kettle, and performing hydrothermal treatment to obtain a black product; cooling the black product, then washing and performing suction filtration on the product, drying, baking in a passivation gas atmosphere, replacing with passivation gas when the temperature is reduced to room temperature, and performing passivation treatment to obtain the nano-molybdenum carbide. The synthesis method provided by the invention has the advantages of simplicity, easiness in control, economical efficiency, reasonableness and large specific surface area with mesoporous structure.

Description

technical field [0001] The invention belongs to the preparation of nanometer materials, in particular to a method for synthesizing rice molybdenum carbide. Background technique [0002] Transition metal carbides are a kind of mesenchymal compound with metallic properties produced by carbon atoms entering the lattice of transition metals. It exhibits the common characteristics of covalent solids, ionic crystals and transition metals, so it has special physical and chemical properties. Properties, specifically manifested as high melting point and hardness, high stability and mechanical stability, and good corrosion resistance. In addition, it has similar electrical and magnetic properties to its parent metal and is widely used in mining, machinery, etc. important industrial fields. Since it was discovered in the 1970s that transition metal carbides have noble metal-like properties in a series of catalytic reactions, transition metal carbides have attracted great attention as ...

Claims

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Application Information

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IPC IPC(8): C01B31/34C01B32/949
Inventor 房克功刘长城韩信有林明桂孙予罕
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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