Preparation method and application of oxidization modified carbon nanotube-loaded double-metal copper and magnesium co-doped nickel-based multi-metal catalyst
A technology of multi-metal catalysts and carbon nanotubes, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as insignificant economic benefits, low recycling rate, and easy deactivation. Achieve high conversion rate and total product selectivity, inhibit excessive hydrogenation, and promote synergistic effect
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Embodiment 1
[0034] First weigh 4g of multi-walled carbon nanotubes and place them in a 350mL round bottom flask, add a corresponding volume of nitric acid mixed acid with sulfuric acid (V (nitric acid) / V (sulfuric acid) = 3) at a liquid-solid ratio of 50 mL / g. In a constant temperature oil bath at 100° C., condense and reflux at a stirring rate of 750 rpm for 10 hours. The carbon nanotubes after the reflux treatment were repeatedly washed 10 times with deionized water until neutral. The washed carbon tubes were put into a vacuum drying oven and dried at a constant temperature of 110° C. for 3 hours. Take 3g of the above-mentioned treated carbon nanotubes and place them in a 150mL round-bottomed flask, and prepare hydrogen peroxide H with a concentration of 1.5mol / L. 2 o 2 solution, add a corresponding volume of H at a liquid-solid ratio of 25 mL / g 2 o 2 , reflux at 40°C for 12 hours. The carbon nanotubes (O-MWCNT) after the oxidation treatment were washed 10 times with a large amount...
Embodiment 2
[0037] Weigh 0.55 g of the oxidation-modified carbon nanotube-supported nickel-based multimetal catalyst (MgO-Cu-Ni / O-MWCNT) catalyst obtained in Example 1 and place it in a 100 mL lining of a high-temperature reactor, add 25 mL of absolute ethanol, Put 2.5 grams of adiponitrile into the magnet, seal the autoclave, replace the air in the autoclave with nitrogen for 4 times, evacuate the autoclave to vacuum with a vacuum pump, and then place the autoclave in an oil bath. After rising to the set reaction temperature of 55°C, hydrogen was introduced to pressurize to 2 MPa, the magnetic stirring was started, the stirring rate was 750rpm, and the reaction timing started. After reacting for 6 hours, the reaction mixture was filtered, and the contents of each substance in the filtrate The content was analyzed by gas chromatography. The conversion rate of adiponitrile was 97.85%, the selectivity of 6-aminocapronitrile was 60.11%, the selectivity of hexamethylenediamine was 32.31%, and...
Embodiment 3
[0039] Weigh 0.55 g of the oxidation-modified carbon nanotube-supported nickel-based multimetal catalyst (MgO-Cu-Ni / O-MWCNT) catalyst obtained in Example 1 and place it in a 100 mL lining of a high-temperature reactor, add 25 mL of absolute ethanol, Put 2.5 grams of adiponitrile into the magnet, seal the autoclave, replace the air in the autoclave with nitrogen for 4 times, evacuate the autoclave to vacuum with a vacuum pump, and then place the autoclave in an oil bath. After rising to the set reaction temperature of 65°C, hydrogen was introduced to pressurize to 2 MPa, the magnetic stirring was started, the stirring rate was 750rpm, and the reaction timing started. After 6 hours of reaction, the reaction mixture was filtered, and the contents of each substance in the filtrate were The content was analyzed by gas chromatography. The conversion rate of adiponitrile was 100%, the selectivity of 6-aminocapronitrile was 20.31%, the selectivity of hexamethylenediamine was 62.98%, a...
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