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Preparation method of 2, 4-dichloroaniline

A technology of dichloroaniline and m-dichlorobenzene, which is applied in the field of preparation of 2.4-dichloroaniline, can solve the problems of low product purity, difficulty in keeping the production environment clean, and high energy consumption, so as to reduce energy consumption and protect the environment Meaning, effect of keeping clean

Inactive Publication Date: 2014-01-15
纪兴国
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Problems solved by technology

At present, 2.4-dichloroaniline is mostly reduced with iron powder in the production process. The purity of the product obtained by iron powder reduction is not high, and it is difficult to keep the production environment clean during the production process, and the energy consumption is large. The country has no advocate this method

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  • Preparation method of 2, 4-dichloroaniline

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Embodiment Construction

[0014] In order to further illustrate the technical solution of the present invention, the preferred embodiments of the present invention are described below in conjunction with examples, but it should be understood that these descriptions are only to further illustrate the features and advantages of the present invention, rather than limiting the claims of the present invention.

[0015] The purity of 2-(4-hydroxyphenoxy)propionic acid, ethanol and toluene used in this example are all ≥99%.

[0016] A preparation method for 2.4-dichloroaniline, comprising the following steps (such as figure 1 shown):

[0017] (1), raw material 160kg sulfuric acid and m-dichlorobenzene are added in the reactor, nitric acid is added dropwise under stirring, nitric acid: m-dichlorobenzene=1: 1.05-1.3 (molar ratio), the temperature in the reactor is controlled at 0- 35°C, the reaction time is 1 hour, after the reaction is completed, the waste acid is filtered off, the product is washed with 1% a...

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Abstract

The invention discloses a preparation method of 2, 4-dichloroaniline. The preparation method comprises the following steps of adding raw materials, namely sulfuric acid and m-dichlorobenzene, into a reaction kettle, dropwise adding nitric acid while stirring, controlling the temperature in the reaction kettle at 0-35 DEG C, filtering waste acid after the reaction is ended, and neutralizing and washing a product to obtain 2, 4-dichloronitrobenzene; adding methanol, 2, 4-dichloronitrobenzene generated in the former step and a composite metal catalyst into the reaction kettle, introducing hydrogen after stirring and heating, and then, recovering methanol to obtain a crude product of 2, 4-dichloroaniline; carrying out filter pressing, vacuum concentration and freezing crystallization to obtain a qualified finished product. A hydrogenation reduction method is adopted in the invention, so that the production link can be effectively kept clean; compared with an iron powder reduction process, the preparation method has the advantages that the vapor distillation is not adopted, so that the energy consumption is effectively reduced, and the better environment-friendly significance is achieved; meanwhile, the purity of a product possibly meets the requirement once.

Description

technical field [0001] The invention relates to a preparation method of an organic synthesis intermediate, in particular to a preparation method of 2.4-dichloroaniline. Background technique [0002] 2.4-Dichloroaniline is mainly used as a synthetic raw material for the anti-infective drug ciprofloxacin, the pesticide fungicide amide azole, herbicides and dyes, and its production and sales ratio is increasing year by year. At present, 2.4-dichloroaniline is mostly reduced with iron powder in the production process. The purity of the product obtained by iron powder reduction is not high, and it is difficult to keep the production environment clean during the production process, and the energy consumption is large. The country has no This method is advocated. Contents of the invention [0003] Aiming at the shortcomings and deficiencies of the prior art, the invention provides a method for reducing 2.4-dichloroaniline by hydrogenation. The invention has simple operation, low...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/36
Inventor 纪兴国
Owner 纪兴国
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