Synthesis of stephanoporate molybdenum carbide nano-wire

A synthesis method and molybdenum carbide technology, applied in the field of nanomaterials, can solve the problems of high cost, cannot be completely eliminated, and high atmosphere requirements, achieve product quality and high yield, good application and industrialization prospects, and simple and easy-to-control preparation conditions. Effect

CN101367521AInactive Publication Date: 2009-02-18FUDAN UNIV
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2009-02-18
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to the technical field of the nanometer material, and relates to a method for synthesizing the porous molybdenum carbide nanometer wire, and adopts the following steps: molybdate is dissolved in the water, and the mol concentration of the molybdenum atom is 0.02 to 1.5 mol / L; organic amine is filled in, and the mol ratio between the organic amine and the molybdenum atom is 20.0 to 1.0: 1; inorganic acid is dropped into the solution, and the pH value is adjusted to be 3 to 6 until the white precipitate appears; the reaction solution is moved into an oil bath with the temperature of 30 to 60 DEG C to be reacted for 6 to 24 hours; (5) the product is washed, pumped, filtered and dried; the product is baked in the inert gases atmosphere at the temperature of 675 to 750 DEG C for 4 to 10 hours. The invention has the advantages that abundant nanometer hole structure is arranged between the nanometer particles, the granularity of the molybdenum carbide is small, the molybdenum carbide has rich porous structure and large specific surface area, the carbon on the surface is small, thereby favoring the secondary assembling of the catalyst and having wide application fields; the productivity can reach 95 percent or more; the conditions are simple and easy to be controlled; the preparation efficiency is high; the invention has favorable application and industrialization prospect.
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Description

technical field

[0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a synthesis method of porous molybdenum carbide nanowires. Background technique

[0002] Transition metal carbide catalysts represented by molybdenum carbide have become the most promising in the past 10 to 20 years because of their unique electronic structure and catalytic performance, anti-sulfur and anti-coking properties, and good thermal stability. one of the catalytic materials. Especially in recent years, with the rapid rise of oil prices, the calls for efficient and green utilization of energy and resources have been increasing, and the development of carbide catalytic performance and new catalytic reactions has further attracted people's attention. In addition, since the raw materials for carbide synthesis are relatively cheap and easy to obtain, it is also of great significance in saving precious metal resources and reducing the cost of catalyti...

Examples

Embodiment 1

[0047] A method for synthesizing porous molybdenum carbide nanowires, characterized in that it comprises the following steps:

[0048] (1) 1.24g ammonium molybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O is dissolved in 20ml distilled water to obtain ammonium molybdate solution (the molar concentration of molybdenum atom is about 0.35mol / L);

[0049] (2) Inject 1.90g of aniline into the ammonium molybdate solution (the molar ratio of aniline to molybdenum atoms is about 2.92:1);

[0050] (3) Add 1.0 mol / L hydrochloric acid dropwise to the solution to adjust the pH to 4-5 until white precipitates appear to obtain a reaction solution;

[0051] (4) The reaction solution was moved to an oil bath at 50°C, and reacted for 6 hours to obtain the product;

[0052] (5) The product was washed several times with absolute ethanol, filtered with suction, and dried at 50°C;

[0053] (6) Finally, the product was calcined in an argon flow at a calcining temperature of 725° C. for a calcining time of...

Embodiment 2

[0060] A method for synthesizing porous molybdenum carbide nanowires, characterized in that it comprises the following steps:

[0061] (1) ammonium molybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O is dissolved in 20ml distilled water to obtain ammonium molybdate solution (the molar concentration of molybdenum atom is 0.02mol / L);

[0062] (2) Inject aniline into the ammonium molybdate solution (the molar ratio of aniline to molybdenum atoms is 4.0-2.0:1);

[0063] (3) Add 1.0 mol / L hydrochloric acid dropwise to the solution to adjust the pH to 4-5 until white precipitates appear to obtain a reaction solution;

[0064] (4) The reaction solution was moved to an oil bath at 50°C, and reacted for 6 hours to obtain the product;

[0065] (5) The product was washed several times with absolute ethanol, filtered with suction, and dried at 50°C;

[0066] (6) Finally, the product was calcined in an argon flow at a calcining temperature of 725° C. for a calcining time of 5 hours to obtain a por...

Embodiment 3

[0068] A method for synthesizing porous molybdenum carbide nanowires, characterized in that it comprises the following steps:

[0069] (1) ammonium molybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O is dissolved in 20ml distilled water to obtain ammonium molybdate solution (the molar concentration of molybdenum atom is 1.5mol / L);

[0070] (2) Inject aniline into the ammonium molybdate solution (the molar ratio of aniline to molybdenum atoms is 4.0-2.0:1);

[0071] (3) Add 1.0 mol / L hydrochloric acid dropwise to the solution to adjust the pH to 4-5 until white precipitates appear to obtain a reaction solution;

[0072] (4) The reaction solution was moved to an oil bath at 50°C, and reacted for 6 hours to obtain the product;

[0073] (5) The product was washed several times with absolute ethanol, filtered with suction, and dried at 50°C;

[0074] (6) Finally, the product was calcined in an argon flow at a calcining temperature of 725°C for a calcining time of 5 hours to obtain a porous...