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Catalyst for recycling phenylamine rectification residue and preparation method of catalyst

A catalyst and resource-based technology, applied in catalyst activation/preparation, organic compound preparation, physical/chemical process catalysts, etc., can solve the problems of high catalyst overall cost, short catalyst life, low economy, etc., and achieve industrial application. , the overall economic improvement, the effect of improving the achievability

Active Publication Date: 2018-05-25
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount consumed by these two uses accounts for a very low proportion of the total amount of aniline distillation residues. Therefore, most of the aniline distillation residues are treated as waste liquids and treated by incineration, but nitrogen oxides will be produced after incineration. Form acid rain, pollute the environment, and reduce the output of agriculture and fishery
[0005] Chinese patent CN201310396100.6 provides a catalyst and its preparation method that can be used for the resource utilization of fixed-bed aniline distillation residues, but it does not have a practical industrial production method
The preparation method of the catalyst reported in this patent is complicated, the feasibility of industrial scale-up is low, and the life of the catalyst is short, which will cause the overall cost of the catalyst to be high
Furthermore, because of the resource utilization of aniline rectification residue, the utilization rate is only 50%-70%, and the economy is low and it is difficult to realize industrial application.

Method used

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  • Catalyst for recycling phenylamine rectification residue and preparation method of catalyst

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Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a catalyst for recycling fixed bed phenylamine rectification residue and a preparation method of the catalyst. The catalyst is prepared from a carrier and an active componentas well as an optional first auxiliary component and second auxiliary component; and the active component is prepared from Ni and Ru, and based on the total weight of the catalyst, the content of Ni is 10 to 40 percent, and the content of Ru is 0.5 to 5 percent. The catalyst has high activity and stability in the process for recycling the fixed bed phenylamine rectification residue, and the yieldof cyclohexane and dicyclohexylamine is high.

Description

technical field [0001] The invention relates to a production method for resource utilization of chemical residues, in particular to a catalyst for resource utilization of aniline rectification residues and a preparation method thereof, and a continuous production method for resource utilization of aniline rectification residues . Background technique [0002] Aniline is a colorless oily liquid with a strong odor and is toxic. It is an important chemical intermediate and is widely used in the production of rubber additives, dyes, photosensitive chemicals, medicines, pesticides, explosives and polyurethanes. Its production methods include phenol ammoniation method, iron powder reduction method and nitrobenzene catalytic hydrogenation method. [0003] Considering the sources of raw materials, energy consumption and environmental protection, most manufacturers adopt the catalytic hydrogenation method of nitrobenzene. The production of aniline by catalytic hydrogenation of nitr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/10B01J23/02B01J23/89C07C209/72C07C211/35
CPCB01J21/10B01J23/02B01J23/894B01J23/8993B01J37/0207B01J37/03C07C209/72C07C211/35B01J21/04B01J23/89Y02P20/584
Inventor 张聪颖李鑫刘振国任树杰陈浩陈忠英倪自林王宁宁邵仁龙张兵王小龙唐磊刘志鹏吴健王丛姜庆梅黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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