Preparation method of Ni-based catalyst modified by aid Pt supported by multi-wall carbon nanotube as carrier and application
A multi-walled carbon nanotube, carrier-loaded technology, applied in the preparation of organic compounds, the preparation of aminohydroxy compounds, chemical instruments and methods, etc., can solve the problems of high requirements for reaction devices, catalyst corrosion, environmental pollution, etc. Mass transfer hindering effect, improving hydrogenation activity and reducing production cost
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Embodiment 1
[0025] First prepare nitric acid mixed acid according to the volume ratio of concentrated nitric acid and concentrated sulfuric acid 3:1. Take 5g of multi-walled carbon nanotubes and place them in a 150mL round bottom flask, add a corresponding volume of nitric acid mixed acid 75mL at a solid-to-liquid mass volume ratio of 1:15g / ml, and stir at 100°C for 16 hours under constant temperature reflux. The carbon nanotubes modified by the mixed acid were repeatedly washed with deionized water until the filtrate was neutral.
[0026]Get 1g of the multi-walled carbon nanotube carrier prepared above, add 0.0218g of chloroplatinic acid hexahydrate, add 0.99g of nickel nitrate hexahydrate, put the above three substances into a 100ml beaker respectively, then add 25ml of deionized water respectively, Under the condition of 25°C, ultrasonically stir for 1h, transfer to a 100ml round bottom flask, stir for 10h at 25°C, pour the stirred solution into a 100ml beaker and put it in a blast dry...
Embodiment 2
[0028] Weigh 0.1g of the Pt-Ni / MWCNT catalyst obtained in Example 1 and place it in a 100mL inner lining of a high-temperature reactor, add 25mL of 15% 1-butyl-3-methylimidazole dihydrogen phosphate aqueous solution, 1.0 g nitrobenzene, 0.03g hexadecyltrimethylammonium bromide, put in a magnet, seal the autoclave, replace the air in the autoclave with nitrogen for 3 times, then disperse under ultrasonic conditions for 1h, and evacuate the autoclave to vacuum with a vacuum pump , and then place the reactor in an oil bath. After rising to the set reaction temperature of 95°C, hydrogen was introduced to pressurize to 1.0 MPa, magnetic stirring was started, and the reaction timing started. After reacting for 4 hours, the temperature was naturally cooled, and the content of each substance in the filtrate was analyzed by liquid chromatography. The conversion rate of nitrobenzene is 94.78%, and the selectivity of p-aminophenol is 53.68%.
Embodiment 3
[0030] Weigh 0.1g of the Pt-Ni / MWCNT catalyst obtained in Example 1 and place it in a 100mL inner lining of a high-temperature reactor, add 25mL of 15% 1-butyl-3-methylimidazole dihydrogen phosphate aqueous solution, 1.0 g nitrobenzene, 0.03g hexadecyltrimethylammonium bromide, put in a magnet, seal the autoclave, replace the air in the autoclave with nitrogen for 3 times, then disperse under ultrasonic conditions for 1h, and evacuate the autoclave to vacuum with a vacuum pump , and then place the reactor in an oil bath. After rising to the set reaction temperature of 105°C, hydrogen was introduced to pressurize to 1.0 MPa, magnetic stirring was started, and the reaction timing started. After reacting for 4 hours, the temperature was naturally cooled, and the content of each substance in the filtrate was analyzed by liquid chromatography. The conversion rate of nitrobenzene is 99.72%, and the selectivity of p-aminophenol is 61.83%.
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