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Preparation method of nanocrystalline metal catalyst loaded with carbon and nitrogen materials

A technology of nano-metal and carbon-nitrogen materials, applied in chemical instruments and methods, physical/chemical process catalysts, amino compound preparation, etc., can solve the problems of increasing reaction conditions, agglomeration deactivation, low activity, etc., and achieve high catalytic performance, Not easy to reunite and not easy to deactivate

Inactive Publication Date: 2014-10-01
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, nanoparticles have a large specific surface area, which makes them extremely unstable and prone to agglomeration and deactivation
In our existing catalytic reactions, there are various complex and diverse reaction conditions. The particles before the catalyst reaction will be agglomerated to a certain extent or even deactivated due to agglomeration, sometimes accompanied by different degrees of loss. Prepare a relatively stable catalyst, but its own activity is not high, so you have to increase the reaction conditions to achieve a higher reaction rate

Method used

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  • Preparation method of nanocrystalline metal catalyst loaded with carbon and nitrogen materials
  • Preparation method of nanocrystalline metal catalyst loaded with carbon and nitrogen materials
  • Preparation method of nanocrystalline metal catalyst loaded with carbon and nitrogen materials

Examples

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Effect test

Embodiment example 1

[0013] Weigh 0.11g of ruthenium (III) chloride hydrate (ruthenium content 37%) in a round bottom flask, 20mL of acetone as solvent, and then add 0.21g of ligand L1 (the molar ratio of metal ruthenium to ligand is 1:2.89) , After stirring at 30° C. for 3 h, 2 g of activated carbon was slowly added. The round bottom flask was heated in an oil bath at 50°C, and after stirring at 50°C for 6h, the solvent acetone was removed by rotary evaporation. The obtained supported pre-catalyst was vacuum-dried at 50° C. for 12 hours. The dried pre-catalyst was placed in a tube furnace and calcined at 800° C. for 2 h under nitrogen (heating rate 4° C. / min). After naturally falling to a constant temperature, a catalyst C1 (with a ruthenium loading of 2%) was obtained.

Embodiment example 2

[0015] Weigh 0.09g rhodium dipolyacetate (rhodium content 46.5%) in a round bottom flask, 20mL ethanol as solvent, then add 0.21g ligand L1 (the molar ratio of metal rhodium to ligand is 1:2.86), and stir at 30°C After 3 h, 2 g of activated carbon was slowly added. The round bottom flask was heated in an oil bath at 60°C, stirred at 50°C for 6h, and then the solvent ethanol was removed by rotary evaporation. The obtained supported pre-catalyst was vacuum-dried at 50° C. for 10 h. The dried pre-catalyst was placed in a tube furnace and calcined at 800°C for 2h under nitrogen (heating rate 4°C / min). After naturally lowering to a constant temperature, catalyst C2 (with rhodium loading of 2.1%) was obtained.

Embodiment example 3

[0017] Weigh 0.08g iridium(III) chloride hydrate (iridium content 52%) in a round bottom flask, 20mL ethanol is used as a solvent, after ultrasonication at room temperature for 3h, add 0.11g ligand L1 (metal iridium and ligand The molar ratio is 1:2.82), then continue stirring at 25°C for 2h, and slowly add 2g of activated carbon. The round bottom flask was heated in an oil bath at 40°C, stirred at 50°C for 5h, and the solvent ethanol was removed by rotary evaporation. The obtained supported pre-catalyst was vacuum-dried at 60° C. for 11 h. The dried pre-catalyst was placed in a tube furnace and calcined at 800°C for 2h under nitrogen (heating rate 4°C / min). After naturally falling to a constant temperature, catalyst C3 (2.1% iridium loading) was obtained.

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Abstract

The invention relates to a preparation method of a nanocrystalline metal catalyst loaded with carbon and nitrogen materials. The preparation method is characterized by comprising the following steps: stirring metal compound and nitrogen-containing ligand in an organic solvent for carrying out coordinating reaction; adding a carrier, heating and stirring; removing the organic solvent; carrying out vacuum drying and finally carrying out calcination under inert gas to obtain the nanocrystalline metal catalyst loaded with the carbon and nitrogen materials. By coordinating metal salt and organic compound, the formation and dispersion of nano metal particles are facilitated; the multi-phase catalyst obtained through calcination has enhanced activity, and is convenient to recycle for repeated use. The preparation method of the catalyst is simple and convenient, raw materials are easily available, and therefore, the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a catalyst, in particular to a method for preparing a nano-metal catalyst supported by a carbon-nitrogen material. Background technique [0002] Nano-scale noble metal catalysts are becoming more and more typical representatives of high-efficiency catalysts and research hotspots in various laboratories and research institutes. However, nanoparticles have a large specific surface area, which makes them extremely unstable and prone to agglomeration and deactivation. In our existing catalytic reactions, there are various complex and diverse reaction conditions. The particles before the catalyst reaction will be agglomerated to a certain extent or even deactivated due to agglomeration, sometimes accompanied by different degrees of loss. A relatively stable catalyst is prepared, but its own activity is not high, so it has to increase the reaction conditions to achieve a higher reaction rate. Therefore, it is...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C211/45C07C209/18C07C209/26C07C43/23C07C41/26
Inventor 黄军耿龙飞汪志黄磊陈华
Owner NANJING UNIV OF TECH
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