Preparation method of catalyst for preparing arylamine from nitro compound through hydrogenation
A technology of nitro compounds and hydrogenation catalysts, which is applied in the preparation of amino compounds, organic compounds, catalyst activation/preparation, etc. It can solve the problems of difficult wastewater treatment, waste of resources, long process flow, etc., to ensure filtration performance, Improve activity and eliminate the effect of internal diffusion
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Embodiment 1
[0046] Weigh 300g of TDI tar residue A, grind it, the average particle size of the tar residue after grinding is 11 μm, and roast the tar residue after grinding at 380°C for 2h in a nitrogen atmosphere for pyrolysis treatment (NH4 is generated during the roasting process. 3 and CO 2 ), cooling to obtain a porous carbon carrier, the carrier content of N element is 0.3%, and the content of Ni element is 0.3%.
[0047] Weigh 0.80g La (NO 3 ) 3 ·6H 2 O, 1.43g Fe(NO 3 ) 3 ·9H 2 O, 19.82g Ni (NO 3 ) 2 ·6H 2 O, 19.91g EDTA in 300ml deionized water, 30wt% ammonia water was slowly added dropwise to the above solution under vigorous stirring, the pH value was adjusted to 8, 5.5g carrier powder was added, and 28KHz was ultrasonically treated at 25°C for 12h, then Dry at 120°C for 12h. A solid powder was obtained, which was refluxed and reduced in a 50 wt% hydrazine hydrate aqueous solution for 2 hours. The reduced catalyst was filtered, washed with deionized water until neutral...
Embodiment 2
[0049] Weigh 300g of TDI tar residue B, and roast the tar residue after grinding at 450°C for pyrolysis treatment for 4h in a nitrogen atmosphere (NH is generated during the roasting process. 3 and CO 2 ), cooling to obtain a porous carbon carrier, the carrier content of N element is 0.1%, and the content of Ni element is 0.1%.
[0050] Weigh 0.21g LaCl 3 ·6H 2 O, 0.29g FeCl 3 , 2.21g NiCl 2 , 4.98g of EDTA in 200ml of deionized water, 50wt% ammonia water was slowly added dropwise to the above solution under vigorous stirring, the pH value was adjusted to 8.5, 8.8g of carrier powder was added, and 35°C was ultrasonically treated at 40KHz for 10h, at 150 Dry at ℃ for 24h. The solid powder was obtained, which was refluxed and reduced in a 60 wt% hydrazine hydrate aqueous solution for 3 hours. The reduced catalyst was filtered, washed with deionized water until neutral, and calcined at 300°C for 4 hours in a nitrogen environment to obtain catalyst B. The Ni content of catal...
Embodiment 3
[0052] Weigh 300g of TDI tar residue C, grind it, the average particle size of the tar residue after grinding is 15 μm, and roast the tar residue after grinding at 600°C for 0.5h in a nitrogen atmosphere for pyrolysis treatment (NH4 is generated during the roasting process. 3 and CO 2 ), cooling to obtain a porous carbon support, the content of N element in the support is 1%, and the content of Pt element is 0.05%.
[0053] Weigh 0.133g La (NO 3 ) 3 ·6H 2 O, 3.61g Fe(NO 3 ) 3 ·9H 2 O, 0.33g PdCl 2 , 0.80gH 2 PtCl 6 ·6H 2 O, 1.55g CrDTA in 300ml deionized water, 30wt% ammonia water was slowly added dropwise to the above solution under vigorous stirring, the pH value was adjusted to 8, 8.9g carrier powder was added, and 30°C was ultrasonically treated at 34KHz for 12h. Dry at 120°C for 12h. The solid powder was obtained, which was refluxed and reduced in a 55 wt% hydrazine hydrate aqueous solution for 2 hours. The reduced catalyst was filtered, washed with deionized w...
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