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Preparation method of carbon onion loaded transition metal carbide nano composite

A technology of nanocomposites and transition metals, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., to achieve the effects of simple preparation process, low energy consumption, and easy operation

Inactive Publication Date: 2012-07-25
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The problem to be solved by the present invention is to overcome the multi-step process of salt decomposition, oxide carbonization and carbide passivation in the existing method in the process of preparing carbon and carbide composites, and to provide an onion carbon with simple process Preparation method of supported transition metal carbide nanocomposite

Method used

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  • Preparation method of carbon onion loaded transition metal carbide nano composite
  • Preparation method of carbon onion loaded transition metal carbide nano composite
  • Preparation method of carbon onion loaded transition metal carbide nano composite

Examples

Experimental program
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specific Embodiment approach 1

[0015] Weigh 2.5 grams of nitrophenol or nitrotoluene, 0.45 grams of cyclohexane or methylcyclohexane and 0.08 grams of ammonium molybdate or 0.12 grams of molybdenum chloride or 0.2 grams of molybdenum nitrate, fully grind in a mortar, and mix well Finally, put it into the high-pressure reactor and tighten the lid of the kettle. Program the temperature from room temperature to 350°C at a rate of 20°C / min to stop heating. The pressure in the reaction kettle is increased to 20-40 MPa. After the pressure in the reaction kettle decreases and the kettle body cools down naturally, the gas product is released and the solid product is collected. The collected sample weighs about 0.2-0.3 grams.

[0016] Characteristic analysis of the sample prepared by the method of the invention shows that the sample is a nanocomposite of carbon and transition metal molybdenum carbide. Directly take a small amount of nanocomposites, disperse them in absolute ethanol and ultrasonically for 15min, dro...

specific Embodiment approach 2

[0017] Weigh 2.5 grams of nitrophenol or nitrotoluene, 0.45 grams of cyclohexane or methylcyclohexane and 0.13 grams of ammonium molybdate or 0.2 grams of molybdenum chloride or 0.32 grams of molybdenum nitrate, fully grind in a mortar, and mix well Finally, put it into the high-pressure reactor and tighten the lid of the kettle. Program the temperature from room temperature to 350°C at a rate of 20°C / min to stop heating. The pressure in the reactor is increased to 20-40 MPa. After the pressure in the reactor decreases and the reactor body cools down naturally, the gaseous product is released and the solid product is collected. The obtained sample weighs about 0.2-0.3 grams. Characterized by high-resolution transmission electron microscopy and X-ray diffractometer, the sample is a nanocomposite of molybdenum carbide supported on onion carbon. The particle size distribution range of onion carbon is 20-30nm. The metal molybdenum carbide dispersed on the surface of onion carbon h...

specific Embodiment approach 3

[0018] Weigh 2.5 grams of nitrophenol or nitrotoluene, 0.45 grams of cyclohexane or methylcyclohexane and 0.18 grams of ammonium molybdate or 0.28 grams of molybdenum chloride or 0.45 grams of molybdenum nitrate, fully grind in a mortar, and mix well Finally, put it into the high-pressure reactor and tighten the lid of the kettle. Program the temperature from room temperature to 350°C at a rate of 20°C / min to stop heating. The pressure in the reactor is increased to 20-40 MPa. After the pressure in the reactor decreases and the reactor body cools down naturally, the gaseous product is released and the solid product is collected. The obtained sample weighs about 0.2-0.3 grams. High-resolution transmission electron microscope and X-ray diffractometer are used to characterize, the sample is the nanocomposite of molybdenum carbide supported on onion carbon, and the particle size distribution range of onion carbon is 30-40nm.

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Abstract

The invention provides a preparation method of a carbon onion loaded transition metal carbide nano composite, comprising the following steps of: uniformly mixing reactant in proportion and then loading the reactant into a closed reaction kettle, wherein a hydrocarbon compound, molybdenum salt or tungsten salt and a nitrocompound are taken as raw materials; and heating the reaction kettle and utilizing a chemical vapor deposition method assisted by an initiator to react for one time to obtain a target product. The preparation method disclosed by the invention has the advantages of simple process and equipment, convenience for operation, fast reaction speed and low energy consumption; the output of the carbon onion and the transition metal carbide nano composite is great, the grain diameter of a carbon onion carrier is controllable, the metal carbide has small granularity and is dispersed uniformly; and the composite is used as a catalyst in a catalyzing field or is used as an additive of a lubricant in a friction field, so as to have an important application value.

Description

technical field [0001] The invention relates to a preparation method of onion carbon-loaded transition metal carbides, specifically cyclohexane or methylcyclohexane and ammonium molybdate, molybdenum chloride, molybdenum nitrate, tungsten chloride, tungsten carbonyl or tungsten A method for preparing an onion carbon-loaded transition metal carbide nanocomposite with acid as a raw material and nitrophenol or nitrotoluene as a reaction initiator is mainly used in the fields of catalysis and friction. Background technique [0002] Since the discovery of fullerenes, fullerene-based carbon materials have attracted widespread attention due to the unique electronic properties of the carbon structure of closed cage molecules. Onion carbon or onion-like fullerene, this carbon structure was first discovered by Ugarte in 1992 (Nature.1992, 359(22):707). Onion carbon is a concentric graphite sheet structure composed of fullerenes with different particle sizes. This unique structure is ...

Claims

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Application Information

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IPC IPC(8): B01J27/22B01J35/02
Inventor 杜建平卫英慧赵瑞花李开喜陈津
Owner TAIYUAN UNIV OF TECH
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