A metal-free hydrogenation catalyst and its application in catalyzing the hydrogenation reaction of 1,5-dinitronaphthalene
A hydrogenation catalyst and dinitronaphthalene technology are applied in physical/chemical process catalysts, preparation of organic compounds, organic chemistry, etc., and can solve the problems of low reaction temperature, loss of metal, increase in catalytic cost, etc., and achieve a simple preparation method. , Low production cost, good hydrogenation effect
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Embodiment 1
[0040] A method for preparing a metal-free hydrogenation catalyst, using melamine as a nitrogen source to prepare nitrogen-doped carbon nanotubes by means of an impregnation method, specifically comprising the following steps:
[0041] (1) Oxidation treatment of carbon nanotubes: carbon nanotubes are acidified by adding a mixed acid of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1 at a solid-to-liquid ratio of 1:80 for acidification for 12 hours, centrifuged and washed, and dried at 80°C for 12 hours Obtain carbon nanotubes.
[0042] (2) Take an appropriate amount of the above-mentioned oxidized carbon nanotubes, mix them with melamine at a mass ratio of 1:1, add deionized water, and add an appropriate amount of formaldehyde twice the mass of melamine, and immerse for 12 hours;
[0043] (3) Add 1mol / L NaOH dropwise to the above solution to adjust the pH to about 10;
[0044] (4) Raise the temperature to 75°C for 30 minutes;
[0045] (5) A...
Embodiment 2
[0049] A method for preparing a metal-free hydrogenation catalyst, using melamine as a nitrogen doping agent to prepare nitrogen-doped carbon nanotubes by an impregnation method, specifically comprising the following steps:
[0050] (1) Oxidation treatment of carbon nanotubes: carbon nanotubes were acidified by adding a mixed acid of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1 at a solid-to-liquid ratio of 1:60 for 15 hours, centrifuged and washed, and dried at 100°C for 12 hours Obtain carbon nanotubes.
[0051] (2) Take an appropriate amount of the above-mentioned oxidized carbon nanotubes, mix them with melamine at a mass ratio of 1:1.1, add deionized water, and add an appropriate amount of formaldehyde three times the mass of melamine, and immerse for 10 hours;
[0052] (3) Add 0.5mol / L KOH dropwise to the above solution to adjust the pH to about 11;
[0053] (4) Raise the temperature to 70°C for 60 minutes;
[0054] (5) After cooli...
Embodiment 3
[0058] A method for preparing a metal-free hydrogenation catalyst, using melamine as a nitrogen doping agent to prepare nitrogen-doped carbon nanotubes by an impregnation method, specifically comprising the following steps:
[0059] (1) Oxidation treatment of carbon nanotubes: carbon nanotubes are acidified by adding a mixed acid of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1 at a solid-to-liquid ratio of 1:120 for 8 hours, centrifuged and washed, and dried at 80°C for 12 hours Obtain carbon nanotubes.
[0060] (2) Take an appropriate amount of the above-mentioned oxidized carbon nanotubes, mix them with melamine at a mass ratio of 1:1.2, add deionized water, and add an appropriate amount of formaldehyde twice the mass of melamine, and immerse for 20 hours;
[0061] (3) Add 2mol / L NaCO dropwise to the above solution 3 , adjust the pH to about 12;
[0062] (4) Raise the temperature to 80°C for 30 minutes;
[0063] (5) After cooling to r...
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