Preparation method of supported catalyst with high specific surface area and application of supported catalyst in paranitroaniline synthesis
A supported catalyst and high specific surface area technology, which is applied in the preparation of organic compounds, catalytic reactions, amino compound preparation, etc., can solve the problems of large usage, low production efficiency, and poor reliability, and achieve large specific surface area and adsorption Good, simple operation effect
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Embodiment 1
[0025] (1) Disperse 10 g of porous nano-silica in 500 ml of deionized water, then add 75 ml of aniline monomer under ice-water bath conditions, mix well and add 50 ml of ammonium persulfate solution with a concentration of 1 mol / L, stir and react at 3000 rpm for 7 hours, and react After the end, the reaction solution was filtered, and the precipitate was washed with deionized water, dried, and the dried solid was placed in an inert atmosphere in a muffle furnace, and the temperature was first raised to 500°C at a rate of 4°C / min, kept for 2 hours, and then heated at 1°C The rate of heating up to 8h at a rate of 1 / min was kept at a temperature of 2h to obtain nano-silicon oxide coated with nitrogen-doped carbon layer;
[0026] (2) Add 5 g of the above-mentioned nano-silicon oxide coated with nitrogen-doped carbon layer to 10 ml of a dispersion of tetrabutylammonium chloride with a concentration of 0.15 g / ml, perform adsorption treatment for 10 h, and then dry at 80° C. 10h, the...
Embodiment 2
[0029] (1) Disperse 10 g of porous nano-silica in 500 ml of deionized water, then add 75 ml of aniline monomer under ice-water bath conditions, mix well and add 50 ml of ammonium persulfate solution with a concentration of 1 mol / L, stir and react at 5000 rpm for 7 hours, and react After the end, the reaction solution was filtered, and the precipitate was washed with deionized water, dried, and the dried solid was placed in an inert atmosphere in a muffle furnace, and the temperature was first raised to 500°C at a rate of 4°C / min, kept for 2 hours, and then heated at 1°C The rate of heating up to 8h at a rate of 1 / min was maintained for 3h to obtain nano-silicon oxide coated with nitrogen-doped carbon layer;
[0030] (2) Add 5 g of the above-mentioned nano-silicon oxide coated with nitrogen-doped carbon layer to 15 ml of a dispersion of tetrabutylammonium chloride with a concentration of 0.15 g / ml, perform adsorption treatment for 10 h, and then dry at 100° C. 10h, the specific...
Embodiment 3
[0033] (1) Disperse 10 g of porous nano-silica in 500 ml of deionized water, then add 75 ml of aniline monomer under ice-water bath conditions, mix well and add 50 ml of ammonium persulfate solution with a concentration of 1 mol / L, stir and react at 3500 rpm for 7 hours, and react After the end, the reaction solution was filtered, and the precipitate was washed with deionized water and dried. The dried solid was placed in an inert atmosphere in a muffle furnace, and the temperature was first raised to 500°C at a rate of 5°C / min, kept for 2h, and then heated at 1°C. The rate of heating up to 8h at a rate of 1 / min was kept at a temperature of 2h to obtain nano-silicon oxide coated with nitrogen-doped carbon layer;
[0034] (2) Add 5 g of the above-mentioned nano-silicon oxide coated with nitrogen-doped carbon layer to 11 ml of a dispersion of tetrabutylammonium chloride with a concentration of 0.15 g / ml, perform adsorption treatment for 115 h, and then dry at 100° C. 20h, the sp...
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