Method for synthesizing phenylamine through nitrobenzene liquid phase continuous hydrogenation

A technology of nitrobenzene liquid and nitrobenzene, which is applied in the field of nitrobenzene liquid-phase continuous hydrogenation to synthesize aniline, and achieves the effects of simple preparation method, high heat transfer coefficient and low loading capacity

Active Publication Date: 2017-11-24
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for directly preparing a supported metal catalyst on the surface of a metal filler with a large specific surface area in view of the shortcomings of the existing liquid-phase hydrogenation method for producing aniline, and then performing continuous liquid-phase nitrobenzene on the surface of the catalyst. Method for synthesizing aniline by hydrogenation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In the first step, put 4L of stainless steel θ ring packing with a specification of 3×3mm into a tubular fixed-bed reactor with a diameter of 100mm and a height of 600mm, and the specific surface area of ​​the packing is 2800m 2 / m 3 , the bulk density is 460kg / m 3 ;

[0025] The second step is to replace the treatment device and pipeline system with nitrogen for 8 to 12 minutes;

[0026] In the third step, chloroplatinic acid and water are mixed and prepared into 150L platinum chloroplatinic acid solution with a platinum concentration of 0.8ppm and put into the solution storage tank as a treatment solution;

[0027] In the fourth step, pump the treatment liquid in the solution storage tank of the third step at a space velocity of 100h -1 Put it into the preheater, the temperature of the preheater is 80°C, and then the space velocity is 500h -1 , The nitrogen-hydrogen mixed gas with a nitrogen-hydrogen ratio of 10:1 is mixed and enters the first step reactor and act...

Embodiment 2

[0030] In the first step, put 4L of 2×2mm stainless steel θ-ring filler into a tubular fixed-bed reactor with a diameter of 100mm and a height of 600mm, and the specific surface area of ​​the filler is 3700m 2 / m 3 , the bulk density is 576kg / m 3 ;

[0031] The second step is to replace the treatment device and pipeline system with nitrogen for 8 to 12 minutes;

[0032] The 3rd step, chloroplatinic acid and water are mixed and prepared into 150L platinum concentration and are the chloroplatinic acid solution of 1.0ppm and put into the solution storage tank as treatment liquid;

[0033] In the fourth step, pump the treatment liquid in the solution storage tank of the third step at a space velocity of 100h -1 Put it into the preheater, the temperature of the preheater is 80°C, and then the space velocity is 800h -1 , The nitrogen-hydrogen mixed gas with a nitrogen-hydrogen ratio of 10:1 is mixed and then enters the reactor of the first step. The temperature of the reactor is...

Embodiment 3

[0036] In the first step, put 4L zirconium orifice corrugated packing into a tubular fixed-bed reactor with a diameter of 100mm and a height of 600mm, and the specific surface area of ​​the packing is 501m 2 / m 3 , the bulk density is 325kg / m 3 ;

[0037] The second step is to replace the treatment device and pipeline system with nitrogen for 8 to 12 minutes;

[0038] In the third step, chloroplatinic acid and water are mixed and prepared into 150L platinum chloroplatinic acid solution with a platinum concentration of 0.5ppm and put into the solution storage tank as a treatment solution;

[0039] In the fourth step, pump the treatment liquid in the solution storage tank of the third step at a space velocity of 100h -1 Put it into the preheater, the temperature of the preheater is 150°C, and then the space velocity is 800h -1 The nitrogen-hydrogen mixed gas with a nitrogen-hydrogen ratio of 10:1 is mixed and then enters the reactor of the first step and acts on the surface ...

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Abstract

The invention discloses a method for synthesizing phenylamine through nitrobenzene liquid phase continuous hydrogenation. The method comprises the following steps: exchanging nitrogen with a reactor filled with an active metal/metal packing catalyst for 8-12 minutes, heating the reactor to 60-200 DEG C, and continuously introducing nitrobenzene and hydrogen which are respectively preheated to 40-120 DEG C into the reactor for a reaction, wherein the liquid space velocity of the nitrobenzene is 0.01-3h<-1>, the gas space velocity of the hydrogen is 100-2000h<-1>, and the pressure in the reactor is 0.3-2.0MPa; condensing a gas-liquid mixture discharged from the reactor by a condenser, and feeding back the hydrogen into the reactor, thereby obtaining a liquid phase, namely a reaction product phenylamine. The active metal catalyst used in the method is high in active metal utilization rate, good in activity, large in heat and mass transfer surface area, small in resistance, free of diffusion influence in the reaction process, high in reaction speed, simple in equipment and production process and high in production efficiency, and can be operated for a long time stably.

Description

technical field [0001] The invention belongs to the field of catalytic reactions, and in particular relates to a method for preparing a supported active metal / metal filler catalyst by using metal filler as a carrier, and then using the catalyst to carry out liquid-phase continuous hydrogenation of nitrobenzene to synthesize aniline. Background technique [0002] Aniline is an important organic chemical intermediate, which is widely used in the production of polyurethane raw material diphenylmethane diisocyanate (MDI), fuel, medicine, rubber additives, pesticides and fine chemical intermediates, with great market potential. At present, nitrobenzene (NB) catalytic hydrogenation is the most used process route for aniline production, accounting for about 85% of the total aniline production capacity. Industrial nitrobenzene catalytic hydrogenation methods include fixed-bed catalytic hydrogenation, fluidized-bed catalytic hydrogenation and liquid-phase hydrogenation. Ni-based or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/46C07C209/36B01J23/42B01J23/46B01J37/18
Inventor 王淑芳侯朋晨任小亮王延吉张东升
Owner HEBEI UNIV OF TECH
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