Preparation method of nitrogen-modified carbon-supported noble metal hydrogenation catalyst and application of catalyst in hydrogenation reaction of pyridine ring compounds
A hydrogenation catalyst, precious metal technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as unfriendly environment, and achieve the effect of simple preparation
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Embodiment 1-8
[0040] Embodiment 1-8: activated carbon pretreatment
[0041] Evenly disperse 1.0g of activated carbon into 25.0mL of treatment agent solution, put its suspension in a 50mL round bottom flask, and gradually raise the temperature to 80°C under constant stirring with a magnetic stirrer at a constant temperature for 10 hours, during which time it will be condensed and condensed with alkali The liquid absorbs the exhaust gas. Then, the suspension was cooled to room temperature, filtered with suction, washed with deionized water several times until the pH value was neutral, and then placed in a vacuum oven at 110°C for 5 hours.
[0042] Place part of the above-mentioned pretreated activated carbon samples in a flowing argon atmosphere, gradually increase the temperature from room temperature to 500-800 °C at a rate of 10 °C / min, keep at the target temperature for 2 hours, and then gradually reduce to room temperature, argon The samples were taken out under air atmosphere and seale...
Embodiment 10
[0051] 1) Normalized selective treatment of carbon surface groups
[0052] Disperse 1.0g of activated carbon evenly into 25.0mL of 30wt% sodium chlorate solution, place the suspension in a 50mL round-bottomed flask, and gradually raise the temperature to 95°C under constant stirring with a magnetic stirrer at a constant temperature for 5 hours, during which time Condensate and absorb tail gas with lye. Then, the suspension was cooled to room temperature, filtered with suction, washed with deionized water several times until the pH value was neutral, and then placed in a vacuum oven at 120°C for 5 hours.
[0053] Place the above-mentioned pretreated activated carbon sample in a flowing argon atmosphere, gradually raise the temperature from room temperature to 600°C at a rate of 10°C / min, keep it at the target temperature for 5h, and then gradually lower it to room temperature, under the argon atmosphere Take out the sample and keep it sealed.
[0054] 2) Condensation reaction...
Embodiment 25
[0077] Add 100g of N-benzyl-2,3-pyridinedicarboximide and 0.1g of the catalyst of Example 10 into a 500mL high-pressure reactor, close the reactor, replace the air in the reactor with nitrogen, then replace the nitrogen with hydrogen, and open the Stirring, the stirring speed is 1400r / min, the reaction temperature is maintained at 50°C, and the hydrogen pressure is 1.0MPa to carry out the reaction. When the content of N-benzyl-2,3-pyridinedicarboximide was detected to be 0 by chromatography, the reaction was stopped and the catalyst was filtered. The filtrate is the product after phase separation, water separation and dehydration by vacuum distillation. Quantitative analysis (molar percentage) by chromatography shows that the conversion rate of hydrogenation reaction is 100%, and the selectivity is 100%. The reaction time is 25min.
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