Raney nickel catalytic preparation method of 2,2'-bipyridine
A catalytic preparation, Raney nickel technology, applied in the direction of organic chemistry, etc., can solve the problems of staying, unable to achieve large-scale production, low reaction yield, etc., to avoid waste, good economic and social benefits, and simple operation. Effect
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[0019] Example 1: First add 1000Kg of pyridine to the evaporation kettle, and add 150Kg of activated Raney nickel catalyst to the reactor. Slowly heat the pyridine in the evaporation kettle to 115°C. The pyridine vapor rises to the cooling tower and turns into droplets and returns to the reactor. The liquid level in the reactor gradually rises. Turn on the stirrer and heating mantle of the reactor to adjust The temperature of the heating jacket is 110~113℃. After the reaction was carried out for 15 hours, 20Kg of Raney nickel catalyst was added to the reactor, and the reaction was continued for 10 hours; another 15Kg of Raney nickel catalyst was added to the reactor, and the reaction was stopped for 8 hours. The reaction liquid was distilled under reduced pressure, 800Kg of petroleum ether was added to the distillation residue and the temperature in the kettle was reduced to 45°C, then the petroleum ether mixture was filtered, and the filtrate was distilled to dryness to obtain...
Example Embodiment
[0020] Example 2: 1300Kg of pyridine was first added to the evaporation kettle, and 220Kg of activated Raney nickel catalyst was added to the reactor. Slowly heat the pyridine in the evaporation kettle to 115°C. The pyridine vapor rises to the cooling tower and turns into droplets and returns to the reactor. The liquid level in the reactor gradually rises. Turn on the stirrer and heating mantle of the reactor to adjust The temperature of the heating jacket is 112~114℃. After the reaction was carried out for 15 hours, 22Kg of Raney nickel catalyst was added to the reactor, and the reaction was continued for 10 hours. Then add 20Kg of Raney nickel catalyst to the reactor and continue the reaction for 8.5 hours to stop. The reaction liquid was distilled under reduced pressure, 1000Kg of petroleum ether was added to the distillation residue and the temperature in the kettle was reduced to 40°C, then the petroleum ether mixture was filtered, and the filtrate was distilled to drynes...
Example Embodiment
[0021] Example 3: 1700Kg of pyridine was first added to the evaporation kettle, and 300Kg of activated Raney nickel catalyst was added to the reactor. Slowly heat the pyridine in the evaporation kettle to 115°C. The pyridine vapor rises to the cooling tower and turns into droplets and returns to the reactor. The liquid level in the reactor gradually rises. Turn on the stirrer and heating mantle of the reactor to adjust The temperature of the heating jacket is 113 to 114°C. After the reaction was carried out for 15 hours, 32Kg of Raney nickel catalyst was added to the reactor, and the reaction was continued for 10 hours. Then add 30Kg of Raney nickel catalyst to the reactor, continue the reaction for 8 hours and stop. The reaction liquid was distilled under reduced pressure, 1500Kg of petroleum ether was added to the distillation residue and the temperature in the kettle was reduced to 43°C, then the petroleum ether mixture was filtered, and the filtrate was distilled to drynes...
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