Catalyst for resource utilization of aniline rectification residue and preparation method thereof
A catalyst and resource utilization technology, applied in the direction of catalyst activation/preparation, organic compound preparation, physical/chemical process catalysts, etc., can solve the problems of short catalyst life, high overall cost of catalyst, and low economic efficiency, and achieve overall economic efficiency Improvement, realization of industrial application, and improvement of realizability
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Embodiment 1
[0042] Weigh each group of medicines according to the ratio shown in Table 1 and dissolve them in distilled water to obtain five groups of solutions with a concentration of about 2.5 mol / L, which are respectively recorded as solutions A1, A2, A3, A4 and A5. Take the sodium hydroxide that concentration is 7.6mol / L again, record as solution B.
[0043] Heat the water in the precipitation tank to 60°C, and then add the solutions A1 and B into the precipitation tank side by side. During the preparation process, the pH value and precipitation temperature were maintained at 6.5-7.5 and 60°C, respectively. After the precipitation is over, keep the stirring speed and precipitation temperature constant, age for 8 hours, filter and wash until neutral, place the precipitate in an oven at 110°C for 12 hours, and after the drying is complete, roast it in an air atmosphere at 400°C for 4 hours, and Crushed and pulverized to 400-600 mesh to obtain magnesia-modified alumina carrier powder D1...
Embodiment 2
[0049] Prepare 80ml of nitrate impregnation solution containing 15g Ni, 0.5g Ru, 0.5g Fe, 1g Mo, 1g Zn, 0.5g Re, 0.5g Ce, pour 81g carrier Z1 into the above impregnation solution, and absorb at room temperature for 2h, the solution Almost completely absorbed. After the above-mentioned adsorbed carrier Z1 is dried, it is calcined at about 475°C for 12 hours, cooled, and then reduced and activated at about 350°C under a reducing atmosphere. , Fe 0.5wt%, Mo 1wt%, Zn1wt%, Re 0.5wt% and Ce 0.5wt% catalyst C1.
[0050] Fill the catalyst C1 with a random volume of 10ml in the fixed-bed reactor; mix liquid ammonia and aniline rectification residue according to the volume ratio of 1:2 to obtain a diluent, adjust the reaction temperature to 150°C, and the system pressure (absolute pressure, The same below) rise to 15MPa and start to feed, diluent space velocity is 0.3h -1 , H 2 The flow rate was 200ml / min, and sampling and analysis began after 10 hours of reaction. The contents of cy...
Embodiment 3
[0052] Prepare 75ml of nitrate impregnation solution containing 10g Ni, 3g Ru, 0.5g Fe, 0.5g Cr, 5g Cu and 5g Zr, pour 76g carrier Z1 into the above impregnation solution, and absorb for 2 hours at room temperature, the solution is basically completely absorbed. After the above-mentioned adsorbed carrier Z1 is dried, it is calcined at about 500°C for 10 hours, cooled, and then reduced and activated at about 400°C under a reducing atmosphere. Catalyst C2 with Cr 1 wt%, Cu 5 wt% and Zr 5 wt%.
[0053] Fill the catalyst C2 with a random volume of 10ml in the fixed-bed reactor; mix methylamine and aniline rectification residue according to the volume ratio of 1:1 to obtain a diluent, adjust the reaction temperature to 200 ° C, and the system pressure (absolute pressure, The same below) rise to 15MPa and start to feed, diluent space velocity is 1.0h -1 , H 2 The flow rate was 300ml / min, and sampling and analysis began after 10 hours of reaction. The contents of cyclohexylamine an...
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