Preparation of nitrogen-modified carbon-supported noble metal hydrogenation catalysts and their application in the hydrogenation of halogenated nitrobenzenes
A technology of hydrogenation catalyst and halogenated nitrobenzene, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, preparation of amino compounds, etc. It can solve the problems of unfriendly environment, achieve green process and fast hydrogenation reaction rate , the effect of inhibiting side effects
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Embodiment 1-6
[0040] Embodiment 1-6: activated carbon pretreatment
[0041] Evenly disperse 1.0g of activated carbon into 25.0mL of treatment agent solution, put its suspension in a 50mL round bottom flask, and gradually raise the temperature to 50°C under constant stirring with a magnetic stirrer at a constant temperature for 15 hours, during which time it will be condensed in circulation and mixed with alkali The liquid absorbs the exhaust gas. Then, the suspension was cooled to room temperature, filtered with suction, washed with deionized water several times until the pH value was neutral, and then placed in a vacuum oven at 110° C. for 5 h.
[0042] The obtained samples were obtained from literature ((a) J.L.Figueiredo, M.F.R.Pereira, M.M.A.Freitas, J.J.M.Orfao, Carbon 1999, 37, 1379-1389; (b) J.Xu, J.Zhao, J.Xu, T.Zhang, X. Li, X.Di, J.Ni, J.Wang, J.Cen, Ind Eng Chem Res 2014, 53, 14272-14281; (c) L.M. Jiayun Li, Xiaoian Li, Chunshan Lu, and Huazhang Liu, Ind.Eng .Chem.Res 2005,44,5...
Embodiment 7
[0048] 1) Normalized selective treatment of carbon surface groups
[0049] Evenly disperse 1.0g of activated carbon into 25.0mL of 20wt% hydrogen peroxide treatment reagent solution, place the suspension in a 50 mL round bottom flask, and gradually raise the temperature to 35°C under constant stirring with a magnetic stirrer at a constant temperature for 15 hours. Circulate condensation and absorb tail gas with lye. Then, the suspension was cooled to room temperature, filtered with suction, washed with deionized water several times until the pH value was neutral, and then placed in a vacuum oven at 110°C for 5 hours.
[0050] 2) Condensation reaction to prepare nitrogen-modified carbon
[0051] Dissolve 10g of ethylenediamine in 30mL of deionized water, gradually add 1.0g of the activated carbon obtained in step 1) under stirring, and after magnetically stirring for 1h, transfer to a 50mL stainless steel hydrothermal kettle, place in an oven, and heat at 250°C, CO 2 Atmosphe...
Embodiment 22
[0072] Add 100g of p-chloronitrobenzene and 0.05g of the catalyst of Example 8 into a 500mL autoclave, close the autoclave, replace the air in the reactor with nitrogen, then replace the nitrogen with hydrogen, start stirring, and the stirring speed is 1400r / min, The reaction was carried out by maintaining the reaction temperature at 50° C. and the hydrogen pressure at 1.0 MPa. When the content of p-chloronitrobenzene was detected to be 0 by chromatography, the reaction was stopped and the catalyst was filtered. The filtrate is the product after phase separation, water separation and dehydration by vacuum distillation. Quantitative analysis (molar percentage) by chromatography shows that the conversion rate of the hydrogenation reaction is 100%, and the selectivity is 99.95%. The reaction time is 45min.
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