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 b

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

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0012] Implementation case 1:

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

Example Embodiment

[0014] Implementation case 2:

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

Example Embodiment

[0016] Implementation case 3:

[0017] Weigh 0.08g of iridium(III) trichloride hydrate (Iridium content 52%) in a round bottom flask, 20mL of ethanol as the solvent, ultrasonic 3h at room temperature, then add 0.11g of ligand L1 (metallic iridium and ligand The molar ratio is 1:2.82), then continue to stir 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 5 hours, and then the solvent ethanol was removed by rotary evaporation. The obtained supported precatalyst was dried under vacuum at 60°C for 11h. The dried pre-catalyst was placed in a tube furnace and calcined at 800°C under nitrogen for 2h (heating rate 4°C / min). After naturally falling to a constant temperature, a catalyst C3 (with an iridium loading of 2.1%) 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

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Claims

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Application Information

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Owner NANJING UNIV OF TECH
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