A nitrogen-doped carbon material-supported cobalt catalyst and its preparation method and application in catalytic oxidation of n-heterocyclic compounds
A nitrogen-doped carbon and cobalt catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of high catalyst production costs, achieve good industrial application prospects, reduce reaction pressure, The effect of reducing the production cost
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Embodiment 1
[0043] Example 1 A nitrogen-doped carbon material-supported cobalt catalyst is prepared by the following method:
[0044] (1) First, 1.868g hexamethylenetetramine (HMT), 5.0g P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer), 1.25g melamine and 3.8g 2,4-Dihydroxybenzoic acid (DA) was dissolved in 150mL H 2 O, then add 1.38mL 1,6-hexanediamine dropwise therein, after the dropwise addition, stir at room temperature for 1h, then transfer to a 200mL hydrothermal kettle, heat up to 130°C in an oven after sealing the hydrothermal kettle, Hydrothermal reaction at this temperature for 4 hours, cooling to room temperature and filtering, the resulting solid was washed with distilled water until neutral, and dried overnight at 70°C in air to obtain a nitrogen-doped carbon material carrier;
[0045] (2) Disperse the nitrogen-doped carbon material support obtained in the above step (1) in a mixture of 0.2g Co(NO 3 ) 2 ·6H 2 In the ammonia solution of O...
Embodiment 2-9
[0057] The application of the nitrogen-doped carbon material loaded cobalt catalyst prepared in Example 1 in the preparation of quinoline compounds by catalytic oxidation of N-heterocyclic compounds, the steps are:
[0058] Add 20 mg of catalyst, 10 mL of solvent and 1 mmol of 1,2,3,4-tetrahydroquinoline into a 25 mL autoclave, then fill the autoclave with O 2 Purging 5 times to completely remove the air therein, after the autoclave was sealed, filled with 10bar O at room temperature 2 , and then heated from room temperature to 130° C., and then reacted at 130° C. with a mechanical stirring speed of 1000 rpm for 4 hours to obtain the product quinoline and its intermediates. After the reaction, the catalyst was collected by centrifugation. The reaction results in different solvents are specifically shown in Table 1:
[0059] Table 1. The results of oxidative dehydrogenation of 1,2,3,4-tetrahydroquinoline in different solvents
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Embodiment 10-18
[0063] According to the operating method and steps of embodiment 4, solvent acetonitrile is used as a fixed solvent, and the reaction times is 4h, respectively changing temperature of reaction, 0 2 Pressure, obtain product quinoline and its intermediate equally, but conversion rate and productive rate are different, specifically as shown in table 2, table 3:
[0064] Table 2. Effect of reaction temperature on the oxidation of 1.1,2,3,4-tetrahydroquinoline
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[0067] Table 3.O 2 Effect of Pressure on Oxidation of 1.1,2,3,4-Tetrahydroquinoline
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