Process for preparing phenylenediamine through micro-reaction technology

A technology of phenylenediamine and micro-reaction, which is applied in the field of preparation of phenylenediamine through micro-reaction technology, which can solve the problems of large heat generation, industrial safety accidents, and large amount of materials, so as to prevent accumulation, controllable process safety, and increase the probability of collision Effect

Active Publication Date: 2020-06-19
江苏方圆芳纶研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many problems in the catalytic hydrogenation method that react instantaneously, generate a lot of heat, and are prone to industrial safety accidents.

Method used

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  • Process for preparing phenylenediamine through micro-reaction technology
  • Process for preparing phenylenediamine through micro-reaction technology
  • Process for preparing phenylenediamine through micro-reaction technology

Examples

Experimental program
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Effect test

Embodiment 1

[0054] A process for preparing phenylenediamine through micro-reaction technology, comprising the following steps: metering and continuously feeding nitroaromatics to be reduced, a solvent, a catalyst and hydrogen into a hydrogenation micro-reactor for hydrogenation-reduction reaction.

[0055] The reaction solution obtained in the hydrogenation microreactor enters the hydrogenation aging device for aging, and the end point is when no nitro compounds are detected.

[0056] The nitroaromatics are m-dinitrobenzene.

[0057] The mol ratio of hydrogen and m-dinitrobenzene added in the hydrogenation microreactor is 14:1; the weight ratio of feed is m-dinitrobenzene: solvent (methanol): catalyst (skeleton nickel)=1: 2.5: 0.08; control the temperature in the hydrogenation microreactor to be 60°C and the pressure to be 7MPa.

[0058] Such as Figure 1~3 As shown, the hydrogenation microreactor includes a casing reactor body, and the casing reactor body includes an inner casing 1, an...

Embodiment 2

[0071] A process for preparing phenylenediamine through micro-reaction technology, comprising the following steps: first making a suspension from nitroaromatics to be reduced, a solvent and a catalyst, and then continuously feeding the suspension into a hydrogenation micro In the reactor, hydrogen is continuously fed into the hydrogenation microreactor at the same time to carry out continuous hydrogenation reduction reaction.

[0072] The reaction solution obtained in the hydrogenation microreactor enters the hydrogenation aging device for aging, and the end point is when no nitro compounds are detected.

[0073] The nitroaromatics are a mixture of m-dinitrobenzene and o-dinitrobenzene, and the mass ratio of m-dinitrobenzene and o-dinitrobenzene is 4:1.

[0074] The mol ratio of hydrogen and m-dinitrobenzene added in the hydrogenation microreactor is 10:1; the weight ratio of feed is m-dinitrobenzene: solvent (methanol): catalyst (skeleton nickel)=1: 1.8: 0.06; Control the te...

Embodiment 3

[0078] A process for preparing phenylenediamine through micro-reaction technology, comprising the following steps: first making a suspension from nitroaromatics to be reduced, a solvent and a catalyst, and then continuously feeding the suspension into a hydrogenation micro In the reactor, hydrogen is continuously fed into the hydrogenation microreactor at the same time to carry out continuous hydrogenation reduction reaction.

[0079] The reaction solution obtained in the hydrogenation microreactor enters the hydrogenation aging device for aging, and the end point is when no nitro compounds are detected.

[0080] The nitroaromatics are a mixture of m-dinitrobenzene, p-dinitrobenzene and o-dinitrobenzene, and the mass ratio of m-dinitrobenzene, p-dinitrobenzene and o-dinitrobenzene is 5:1:2 .

[0081] The mol ratio of hydrogen and m-dinitrobenzene added in the hydrogenation microreactor is 12:1; the feed weight ratio is m-dinitrobenzene: solvent (methanol): catalyst (skeleton ...

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Abstract

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a process for preparing phenylenediamine through a micro-reaction technology. The method comprises the following steps: metering to-be-reduced nitro aromatic hydrocarbon, a solvent, a catalyst and hydrogen, continuously feeding into a hydrogenation micro-reactor, and carrying out a hydrogenationreduction reaction, wherein the to-be-reduced nitro aromatic hydrocarbon can also be prepared by adopting a continuous micro-nitrification process. According to the invention, a hydrogenation reduction reaction is carried out by adopting a hydrogenation micro-reactor, so that the process is safe and controllable; and particularly nitro aromatic hydrocarbon is prepared by combining a micro-nitrification reactor, and the material directly enters the hydrogenation micro-reactor without separation, so that the method is a continuous production process containing the micro-reactor, can prevent accumulation of dinitrobenzene in the process, and is an intrinsically safe phenylenediamine preparation process.

Description

technical field [0001] The application belongs to the technical field of fine chemicals, and in particular relates to a process for preparing phenylenediamine through micro-reaction technology. Background technique [0002] Micro-reaction technology generally refers to the continuous flow reaction technology with micro-reactor as the core component. Microreactor (Micro-channel reactor), also known as micro-channel reactor (Micro-channel reactor), is essentially a continuous flow pipeline reactor, the internal channel size is much smaller than the traditional conventional reactor, due to The heat exchange rate of the microreactor is extremely high, even if the reaction suddenly releases a large amount of heat, it can be quickly exported, reducing the possibility of safety accidents and quality accidents to the greatest extent. [0003] The traditional m-phenylenediamine production uses iron powder as a reducing agent to reduce m-dinitrobenzene to m-phenylenediamine in an aci...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/51C07C201/08C07C201/14C07C205/06B01J19/00
CPCC07C209/36C07C201/08C07C201/14B01J19/0093C07C205/06C07C211/51
Inventor 王农跃沙艳松章冬霞李斌许坚
Owner 江苏方圆芳纶研究院有限公司
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