Method for preparing 2-methyl-1,4-naphthoquinone by catalytic oxidation of 2-methylnaphthalene using functionalized carbon materials
A technology for catalytic oxidation and carbon materials, applied in the preparation of quinone oxide, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problems of environmental pollution, low yield, complex process, etc. The effect of high receptivity and convenient preparation process
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Embodiment 1
[0027] Synthesis of functionalized carbon material catalyst: Add 0.45g of thiourea-type benzoxazine monomer into 4mL of tetrahydrofuran, and stir until a clear and uniform solution, then add 0.45g of SBA-15 to the above solution, 60w ultrasonic treatment for 5h . Then the composite is cured by program: 120°C (1h), 140°C (1h), 160°C (1h), 180°C (2h), 200°C (2h), 220°C (1h). The cured compound was placed in a tube furnace, and in a high-purity nitrogen atmosphere, the temperature was raised from room temperature to 400°C at a rate of 2°C / min, and maintained at this temperature for 2h, and then raised to the target temperature of 800°C , and maintained at this temperature for 2h, then cooled to room temperature. The carbonized sample was etched with 50 mL of 50% HF aqueous solution for 24 h, washed with deionized water until neutral, washed with ethanol three times, and finally dried overnight in an oven at 60 °C. The dried product is a thiourea-type benzoxazin-based nitrogen / s...
Embodiment 2
[0031] Synthesis of functionalized carbon material catalyst: Add 0.5g of aniline-type benzoxazine monomer into 4mL of tetrahydrofuran, and stir until a clear and homogeneous solution, then add 0.5g of SBA-15 to the above solution, 60w ultrasonic treatment for 5h . Then the composite is cured by program: 120°C (1h), 140°C (1h), 160°C (1h), 180°C (2h), 200°C (2h), 220°C (1h). The cured compound was placed in a tube furnace, and in a high-purity nitrogen atmosphere, the temperature was raised from room temperature to 400°C at a rate of 2°C / min, and maintained at this temperature for 2h, and then raised to the target temperature of 800°C , and maintained at this temperature for 2h, then cooled to room temperature. The carbonized sample was etched with 50 mL of 50% HF aqueous solution for 24 h, washed with deionized water until neutral, washed with ethanol three times, and finally dried overnight in an oven at 60 °C. The dried product is an aniline-type benzoxazin-based nitrogen-...
Embodiment 3
[0035] Using the carbon material prepared in Example 1 as a catalyst, put 0.3g of 2-methylnaphthalene, 8mL of acetic acid, and 0.1g of catalyst into a three-necked flask, use an oil bath to control the reaction temperature, and use magnetic stirring. At a rotation speed of 550rpm, Slowly add 30% hydrogen peroxide 8mL dropwise, the reaction time is 4h, and then filter the product. The content of the reaction products was analyzed by gas chromatography. The reaction temperature was changed, and the activity was investigated respectively. The results are shown in Table 1.
[0036] Table 1 Catalyst activity comparison under different temperature conditions
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