Preparation method and application of nitrogen-doped activated carbon supported alkali metal modified nickel-based catalyst
A nickel-based catalyst, activated carbon technology, applied in catalyst activation/preparation, amino compound preparation, organic compound preparation and other directions, can solve the problems of complex preparation process, low recovery rate, large hydrogen consumption, etc., and achieves simple preparation process, The effect of reducing production costs and improving production conditions
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Embodiment 1
[0036]Weigh 30g of wood charcoal material, put it in a 1000mL single-neck flask, add 450mL of nitric acid solution with a mass fraction of 50% according to a solid-to-liquid ratio of 1:15, put it in a magnet, and stir in a water bath with a constant temperature of 30°C. (stirring speed is 1000rpm) for 12 hours, the suspension is suction filtered, washed repeatedly with distilled water until neutral, and dried at 100°C for 2 hours to obtain the desired activated carbon material. Weigh the above 10g of activated carbon and place it in a 100mL single-neck flask, add 20ml of deionized water, 10g of melamine, and 20ml of 38% formaldehyde solution by mass, put it into a 75°C oil bath and stir (stirring speed is 1000rpm), while the stirring process Add 5ml of 0.5mol / L NaOH solution, stir (stirring rate is 1000rpm) for 60min; cool the obtained mixture to room temperature, add 5ml of acetic acid, stir (stirring rate is 1000rpm) for 12 hours, centrifuge, filter, at 100 ℃ drying for 10 h...
Embodiment 2
[0039] Weigh 1 gram of the above 1%K-20%Ni / N-AC catalyst and place it in the 100mL lining of the high temperature reaction kettle, add 50mL of absolute ethanol, 5g of adiponitrile, put it into the magnet, seal the autoclave, use nitrogen The air in the autoclave was replaced 4 times, the autoclave was evacuated by a vacuum pump, and then the autoclave was placed in an oil bath. After reaching the set reaction temperature of 70 °C, hydrogen was introduced to pressurize it to 2 MPa, and the magnetic stirring was started (stirring rate was 1000 rpm), and the reaction timing started. After the reaction, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion of adiponitrile was 92.32%, the selectivity of 6-aminocapronitrile was 11.95%, and the selectivity of hexamethylenediamine was 80.36%.
Embodiment 3
[0041] Weigh 1 gram of the above 1%K-20%Ni / N-AC catalyst and place it in the 100mL lining of the high temperature reaction kettle, add 50mL of absolute ethanol, 5g of adiponitrile, put it into the magnet, seal the autoclave, use nitrogen The air in the autoclave was replaced 4 times, the autoclave was evacuated by a vacuum pump, and then the autoclave was placed in an oil bath. After reaching the set reaction temperature of 80 °C, hydrogen was introduced to pressurize it to 2 MPa, and the magnetic stirring was started (stirring rate was 1000 rpm), and the reaction timing started. After the reaction, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion of adiponitrile was 99.49%, the selectivity of 6-aminocapronitrile was 1.12%, and the selectivity of hexamethylenediamine was 86.96%.
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