Method for producing phenylenediamine by solvent-free hydrogenation continuous reaction of dinitrobenzene

A technology for producing phenylenediamine and dinitrobenzene, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problem of reducing the yield of phenylenediamine, high material consumption and energy consumption, and many side reactions to achieve significant economic and social benefits, reduce production material consumption and energy consumption, and reduce by-products

Pending Publication Date: 2020-09-15
四川北方红光特种化工有限公司
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Problems solved by technology

[0004] Due to the need to use methanol or ethanol as a solvent in the reaction, the method requires high material consumption and energy consumption in the process of solvent separation and recovery; under reaction conditions, methanol or ethanol can also alkylate the generated phenylenediamine, thereby reducing Yield of phenylenediamine
[0005] In addition, the invention pate

Method used

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  • Method for producing phenylenediamine by solvent-free hydrogenation continuous reaction of dinitrobenzene
  • Method for producing phenylenediamine by solvent-free hydrogenation continuous reaction of dinitrobenzene

Examples

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Example Embodiment

[0047] Example 1

[0048] A method for producing phenylenediamine by continuous reaction of dinitrobenzene solvent-free hydrogenation, using dinitrobenzene as a raw material to obtain phenylenediamine through continuous hydrogenation reaction, comprising the following steps:

[0049] S1, 100 grams of water, 100 grams of phenylenediamine (wherein, the weight ratio of o-phenylenediamine, m-phenylenediamine and p-phenylenediamine is 1:0.7:0.7, that is, o-phenylenediamine is 40 grams, m-phenylenediamine is 30 grams, and p-phenylenediamine is 30 grams), and 10 grams of Raney nickel is added to the continuous fully mixed flow reactor;

[0050] S2, feeding nitrogen into the continuous fully mixed flow reactor, then circulating hydrogen to carry out displacement and boosting to 2.0MPa, and heating to 120°C;

[0051] S3, continuously drop into dinitrobenzene in the continuous fully mixed flow reactor, carry out hydrogenation reaction;

[0052] S4. The phenylenediamine reducing soluti...

Example Embodiment

[0057] Example 2

[0058] As another embodiment, other features are the same as in Example 1, except that the added amount of phenylenediamine is 90 grams.

[0059] In the present embodiment, taking 1 hour as the experimental time, collecting the phenylenediamine A2 generated within the experimental time, detecting and recording the weight and yield of the phenylenediamine, the relevant data are shown in Table 1.

Example Embodiment

[0060] Example 3

[0061] As another embodiment, the remaining features are the same as in Example 1, except that the added amount of phenylenediamine is 110 grams.

[0062]In the present embodiment, take 1 hour as the experimental time, collect the phenylenediamine A3 generated within the experimental time, detect and record the weight and yield of the phenylenediamine, and the relevant data are shown in Table 1.

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Abstract

The invention provides a method for producing phenylenediamine by solvent-free hydrogenation continuous reaction of dinitrobenzene, which is used for preparing phenylenediamine by continuous hydrogenation reaction of dinitrobenzene as a raw material, and comprises the following steps of: S1, adding water, phenylenediamine and a catalyst into a hydrogenation reactor, and mixing; S2, introducing nitrogen into the hydrogenation reactor, then circularly introducing hydrogen for replacement and pressure rise, and raising the temperature; and S3, continuously adding dinitrobenzene into the hydrogenation reactor, and carrying out a hydrogenation reaction. According to the method for producing phenylenediamine through solvent-free hydrogenation continuous reaction of dinitrobenzene, the yield of phenylenediamine is greatly increased through continuous hydrogenation reaction.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a method for producing phenylenediamine through solvent-free hydrogenation continuous reaction of dinitrobenzene. Background technique [0002] Phenylenediamine is an important raw material for organic synthesis, mainly including three isomers (m-phenylenediamine, o-phenylenediamine and p-phenylenediamine), widely used in the manufacture of azo dyes, oxazine dyes and reactive dyes. Phenylenediamine is mainly obtained from dinitrobenzene by hydrogenation and purification. [0003] The existing public method: using methanol or ethanol as a solvent, mixing water, methanol and catalyst in a certain proportion in a continuous full-mixed flow hydrogenation reactor, at a temperature of 95-105 ° C and a gauge pressure of 2.0 MPa, the hydrogenation reaction Dinitrobenzene is continuously put into the reactor, and the reducing liquid obtained after the reaction of dinitrobenzene and hydro...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C209/86C07C209/84C07C211/51
CPCC07C209/36C07C209/86C07C209/84C07C211/51
Inventor 赖聚黄清武宁萍
Owner 四川北方红光特种化工有限公司
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