A kind of method that nitrogen-doped carbon nanotube catalyzes the oxidation of ethylbenzene to prepare acetophenone
A technology of catalytic oxidation and nanotubes, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of the conversion rate of ethylbenzene and other problems, and achieve low cost, environmental friendliness, and good stability. Effect
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Embodiment 1~4
[0027] Add 20mL of acetonitrile, 0.6g of anisole (internal standard), 2.6g of ethylbenzene, 0.78g of TBHP and 15mg of NCNTs (N content is 3.19at%) into the autoclave and heat it to the temperature shown in Table 1. , feed oxygen, start timing, and maintain its pressure at 1.5MPa during the reaction, and the stirring speed is 1000rpm. After reacting for 4 hours, stop timing, cool the reactor to room temperature, and filter the liquid-solid phase mixture to obtain a solid catalyst and a liquid phase mixture containing unreacted reactants and reaction products. The liquid phase mixture was detected and analyzed by gas chromatography (GC). The gas chromatogram of the reaction solution after the reaction of embodiment 3 is as follows figure 2 shown. The GC detection results are shown in Table 1 (the influence of reaction temperature on the liquid-phase oxidation reaction of ethylbenzene).
[0028] Table 1 Effect of reaction temperature on liquid phase oxidation of ethylbenzene ...
Embodiment 5~9
[0032] Add 20mL of acetonitrile, 0.6g of anisole (internal standard), 2.6g of ethylbenzene, 0.78g of TBHP and 15mg of NCNTs (N content is 3.19at%) into the autoclave in turn, stir and heat, feed in oxygen, and start timing , and maintain its pressure as shown in Table 2 during the reaction process, maintain its temperature at 150° C., and a stirring speed of 1000 rpm. After reacting for 4 hours, stop timing, cool the reactor to room temperature, and filter the liquid-solid phase mixture to obtain a solid catalyst and a liquid phase mixture containing unreacted reactants and reaction products. The liquid phase mixture was detected and analyzed by gas chromatography (GC). The GC detection results are shown in Table 2 (the influence of reaction pressure on the liquid-phase oxidation reaction of ethylbenzene).
[0033] Table 2 Effect of reaction pressure on liquid phase oxidation of ethylbenzene
[0034] Example 5 6 7 8 9 Reaction pressure (MPa) 0.1 1.0 1....
Embodiment 10~13
[0037]Add 20mL of acetonitrile, 0.6g of anisole (internal standard), 2.6g of ethylbenzene, 0.78g of TBHP and 15mg of NCNTs (N content is 3.19at%) into the autoclave in turn, stir and heat, feed in oxygen, and start timing , and maintain its temperature at 150° C. during the reaction, control the stirring speed as shown in Table 3, and the pressure at 1.5 MPa. After reacting for 4 hours, stop timing, cool the reactor to room temperature, and filter the liquid-solid phase mixture to obtain a solid catalyst and a liquid phase mixture containing unreacted reactants and reaction products. The liquid phase mixture was detected and analyzed by gas chromatography (GC). The GC detection results are shown in Table 3 (the influence of stirring speed on the liquid-phase oxidation reaction of ethylbenzene).
[0038] Table 3 Effect of stirring speed on liquid phase oxidation of ethylbenzene
[0039]
[0040]
[0041] Analysis of the data in Table 3 shows that the conversion rate of ...
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