Catalytic agent for preparing p-aminophenol by using nitrobenzene catalytic hydrogenation and preparation method thereof
A technology for p-aminophenol and catalytic hydrogenation, which is used in the preparation of amino hydroxy compounds, the preparation of organic compounds, and metal/metal oxide/metal hydroxide catalysts, etc. problems such as loss, to achieve the effect of good hydrogen absorption, improved activity and selectivity, and good catalytic performance
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Embodiment 1
[0020] Immerse 40-60g of activated carbon purified by nitric acid in 15-20ml of chloroplatinic acid aqueous solution with a volume concentration of 4-8%, keep the temperature at 50°C for 4-6h, and cool to 20°C; prepare saturated aqueous sodium carbonate solution , adjust the impregnation solution to be alkaline; add excess hydrazine hydrate dropwise while stirring, and then keep warm on a water bath for 1-4 hours to completely reduce the chloroplatinic acid; filter the solid phase components, wash with deionized water until there is no chloride ion, Put it in a vacuum dryer and dry it to get 40-60g of Pt / C catalyst, which is for later use; dissolve 8-12g of ammonium tetrathiomolybdate crystal (ATTM) in deionized water, add the spare Pt / C, and stir magnetically under the condition of immersion 1-3h, stand still for 4-8h, and dry at 60-90°C to obtain the catalyst precursor ATTM-Pt / C(I); put ATTM-Pt / C(I) into a quartz tube and place it in a tube furnace Medium roasting, the tempe...
Embodiment 2
[0022] In a stirred reactor at normal pressure, add 100ml of distilled water, 10ml of concentrated sulfuric acid with a mass fraction of 98%, 0.05ml of dimethyl sulfoxide, and 0.3g of MoS 2 - Pt / C catalyst, 20ml nitrobenzene. Pass N 2 , replace the air in the device, and check the airtightness. Heat up to about 87°C, keep the temperature constant, pass H 2 . Stop heating after 5 h of reaction, pass N 2 Purge, cool to room temperature, and recover the catalyst. According to GC-MS analysis, the yield of p-aminophenol is 86%.
Embodiment 3
[0024] Using the catalyst in Example 2, the reaction conditions were the same as above, and after 22 cycles, the yield of p-aminophenol in the 23rd reaction solution was determined to be 83%.
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