Preparation method of fluidized bed catalyst for aniline production by gas phase hydrogenation of nitrobenzene
A fluidized bed catalyst, nitrobenzene gas technology, applied in the preparation of amino compounds, the preparation of organic compounds, catalysts for physical/chemical processes, etc. question
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Embodiment 1
[0050] Boil the recovered electrolytic copper block in 5-10% sodium hydroxide solution for 3 hours, remove the lye, soak in 3% dilute nitric acid or dilute sulfuric acid for 8 hours, remove the acid solution, wash with water until neutral, and obtain Purified copper with a content greater than 99.5% (by weight) is ready for use.
[0051] A 1-liter four-neck flask is equipped with a mechanical stirrer, a thermometer, and a condenser respectively. Add 418 grams of water and 113 grams of glacial acetic acid, and pass ammonia gas under stirring until the pH is greater than 7.0. Add 63.6 grams of the above-mentioned copper block, and pass air and ammonia gas to maintain the temperature Below 70°C, after about 4 hours, add 21.8 grams of the above-mentioned copper block, continue to pass air and ammonia gas until the copper powder reacts completely, about 7 hours, cool, filter to remove a small amount of residue, and obtain cuproammonia liquid (1). After analysis, the total copper co...
Embodiment 2
[0055] The preparation method of copper ammonia liquid (1) is with [embodiment 1].
[0056] Weigh 4.6 grams of Cr(NO 3 ) 3 9H 2 O, 1.2 g Ba(NO 3 ) 2 and 2.7 g of Zn(NO 3 ) 2 ·6H 2 O was dissolved in 450 grams of hot water, 160 grams of silicon dioxide was added while it was hot, stirred for 30 minutes, dried at 100°C for 8 hours, and then calcined at 500°C for 4 hours to obtain the carrier (B).
[0057] A 1-liter three-necked flask is equipped with a thermometer and mechanical stirring, weighs 450 grams of cuproammonia solution (1) and mixes it with the carrier (B), first soaks at 50-60°C for 2 hours, then raises the temperature to 70-80°C for 2 hours, and then Rise to 85-90 ° C for 8 hours, cool, filter, wash twice with 2.5% dilute ammonia water 500 ml, then wash with deionized water until there is no blue color, dry at 100 ° C for 12 hours, and then bake at 400 ° C for 4 hours. Hour. Under the process condition of the present invention, investigation result sees [em...
Embodiment 3
[0059] The preparation method of copper ammonia liquid (1) is with [embodiment 1].
[0060] Weigh 4.6 grams of Cr(NO 3 ) 3 9H 2 O, 1.1 g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 1.2 g Ba(NO 3 ) 2 and 2.7 g of Zn(NO 3 ) 2 ·6H 2 O and 3.0 g Ni(NO 3 ) 2 ·6H 2 O was dissolved in 450 grams of hot water, 160 grams of silicon dioxide was added while it was hot, stirred for 30 minutes, dried at 100°C for 8 hours, and then calcined at 500°C for 4 hours to obtain the carrier (C).
[0061] A 1-liter three-necked flask is equipped with a thermometer and mechanical stirring, weighs 485 grams of cuproammonia solution (1) and mixes it with the carrier (C), first soaks at 50-60°C for 2 hours, then raises the temperature to 70-80°C for 3 hours, and then Rise to 85-90 ° C for 5 hours, cool, filter, wash twice with 2.5% dilute ammonia water 500 ml, then wash with deionized water until there is no blue color, dry at 100 ° C for 12 hours, and then bake at 400 ° C for 4 hours. Hour. Under the p...
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