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
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[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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