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A method for preparing 2,4-dinitrochlorobenzene by one-step adiabatic continuous nitration of chlorobenzene

A one-step technology of dinitrochlorobenzene and chlorobenzene, which is applied in the preparation of nitro compounds, chemical instruments and methods, organic chemistry, etc., can solve problems such as energy consumption, improve production efficiency, space-time efficiency, and rapid heat exchange capacity. , to avoid the effect of side reactions

Active Publication Date: 2022-02-08
DONGYING ANNUOQI TEXTILE MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the inventor has found through research that this method of using a microreactor needs to adopt heat exchange to control the reaction temperature. During heat exchange, a large amount of cooling medium is required to cool the microreactor, and the preparation of the cooling medium requires energy consumption, so the method has energy higher disadvantage

Method used

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  • A method for preparing 2,4-dinitrochlorobenzene by one-step adiabatic continuous nitration of chlorobenzene
  • A method for preparing 2,4-dinitrochlorobenzene by one-step adiabatic continuous nitration of chlorobenzene
  • A method for preparing 2,4-dinitrochlorobenzene by one-step adiabatic continuous nitration of chlorobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Mix 98% sulfuric acid and 98% nitric acid in a mass ratio of 12:1 to prepare a sulfuric acid solution of nitric acid, and store it in the mixed acid storage bottle A.

[0053] (2) Prepare an oil phase solution with chlorobenzene and 2,4-dinitrochlorobenzene at a mass ratio of 1.5:1, and store it in oil phase storage bottle B.

[0054] (3) The sulfuric acid solution of nitric acid and chlorobenzene (according to the molar ratio of nitric acid and chlorobenzene: 2.02:1) are respectively transported to the microreactor D using a high-precision high-pressure plunger pump C, and the inlet temperature is 30°C. The reaction was carried out under the following conditions, the reaction residence time was 70 seconds, and the temperature sensor detected an outlet temperature of 125°C.

[0055] (4) The reacted reaction solution flows into the reaction solution storage bottle H.

[0056] (5) After the reaction solution is cooled to 80°C, take out 20mL of the reaction solution f...

Embodiment 2

[0059] The operating process is the same as in Example 1, only changing the mol ratio of nitric acid and chlorobenzene to 2.04:1, and the gas chromatography detection results are: mononitrochlorobenzene (0.2%), 2,4-dinitrochlorobenzene (99.8%) .

Embodiment 3

[0061] The operating process is the same as in Example 1, only changing the mol ratio of nitric acid and chlorobenzene to 2.06:1, and the gas chromatography detection results are: 2,4-dinitrochlorobenzene (99.7%), trinitrochlorobenzene (0.3%) .

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Abstract

The invention discloses a method for preparing 2,4-dinitrochlorobenzene by one-step adiabatic and continuous nitration of chlorobenzene. A mixed acid solution and an organic phase solution are added to a microreactor for adiabatic nitration reaction to obtain 2,4-dinitrochlorobenzene Chlorobenzene; Wherein, described mixed acid solution is the mixture of concentrated sulfuric acid and concentrated nitric acid; Described organic phase solution is the mixture of chlorobenzene and heat carrier, and described heat carrier is 2,4-dinitrochlorobenzene; A micro-sieve structure is set inside the reactor. The method of the invention has the advantages of greenness, energy saving and high efficiency at the same time.

Description

technical field [0001] The invention belongs to the technical field of chemical production and relates to a synthesis method of 2,4-dinitrochlorobenzene, in particular to a method for preparing 2,4-dinitrochlorobenzene by one-step adiabatic continuous nitration of chlorobenzene. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] 2,4-Dinitrochlorobenzene is an important fine chemical intermediate, which is widely used in medicine, pesticides, dyes, explosives, chemical auxiliaries and other fields. Many important fine chemical intermediates can be derived downstream. The main varieties There are 2,4-dinitroaniline, 2,4-dinitrophenol, 2,4-diaminochlorobenzene, 2,4-diaminopheno...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/08C07C205/12B01J19/00
CPCC07C201/08B01J19/0093C07C205/12
Inventor 骆广生邓建刘云龙乔鹏伟张建军冯全明吴劲于子航王海任李建华
Owner DONGYING ANNUOQI TEXTILE MATERIALS
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