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

A one-step technology of dinitrochlorobenzene and chlorobenzene, which can be used in the preparation of nitro compounds, chemical instruments and methods, organic chemistry, etc., and can solve problems such as energy consumption

Active Publication Date: 2021-04-27
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...

Method used

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  • Method for preparing 2, 4-dinitrochlorobenzene by one-step adiabatic continuous nitration of chlorobenzene
  • Method for preparing 2, 4-dinitrochlorobenzene by one-step adiabatic continuous nitration of chlorobenzene
  • 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) 98% sulfuric acid and 98% nitric acid are prepared into a sulfuric acid solution of nitric acid in a mass ratio of 12:1, and stored in a mixed acid storage bottle A.

[0053] (2) chlorobenzene and 2,4-dinitrochlorobenzene are prepared into oil phase solution by mass ratio of 1.5:1, and stored 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, under adiabatic conditions The reaction was carried out under the following conditions, the reaction residence time was 70 seconds, and the temperature sensor detected the outlet temperature of 125°C.

[0055] (4) The reaction liquid after the reaction flows into the reaction liquid storage bottle H.

[0056] (5) After the reaction solution is cooled to 80°C, take o...

Embodiment 2

[0059] The operation process is the same as in Example 1, except that the molar ratio of nitric acid and chlorobenzene is changed to 2.04:1, and the gas chromatography detection result is: mononitrochlorobenzene (0.2%), 2,4-dinitrochlorobenzene (99.8%) .

Embodiment 3

[0061] The operation process is the same as in Example 1, except that the molar ratio of nitric acid and chlorobenzene is changed to be 2.06:1, and the gas chromatography detection result is: 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 continuous nitration of chlorobenzene, which comprises the following steps: adding a mixed acid solution and an organic phase solution into a microreactor for adiabatic nitration reaction to obtain 2, 4-dinitrochlorobenzene, wherein the mixed acid solution is a mixture of concentrated sulfuric acid and concentrated nitric acid. The organic phase solution is a mixture of chlorobenzene and a heat carrier, and the heat carrier is 2, 4-dinitrochlorobenzene; and a micro-sieve pore structure is arranged in the micro-reactor. The method provided by the invention has the advantages of greenness, energy conservation and high efficiency.

Description

technical field [0001] The invention belongs to the technical field of chemical production and relates to a method for synthesizing 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 for enhancement of understanding of the general background of the invention and should not necessarily be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. [0003] 2,4-Dinitrochlorobenzene is an important fine chemical intermediate, which is widely used in medicine, pesticides, dyes, explosives, chemical additives 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-diaminoph...

Claims

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Application Information

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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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