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2-4-dichloronitrobenzene synthesis method utilizing micro-channel reactor

A technology of microchannel reactor and dichloronitrobenzene, which is applied in the preparation of nitro compounds and organic chemistry to achieve the effects of ensuring safety, improving selectivity and improving production efficiency

Active Publication Date: 2015-04-01
ZHEJIANG YONGTAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The use of microchannel reactors to carry out the nitration of m-dichlorobenzene to synthesize 2,4-dichloronitrobenzene has not been reported in the literature

Method used

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Experimental program
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Effect test

Embodiment 1

[0032] (1) Device: Corning high-throughput microchannel reactor. The reactor is configured as image 3 As shown, microchannel reactor 1-4 is the first temperature zone, microchannel reactor 5-6 is the second temperature zone, and microchannel reactor 4 is supplemented with mixed acid feed. Microchannel reactor 1-2 is used for precooling mixed acid and m-dichlorobenzene.

[0033] (2) prepare mixed acid according to mass ratio nitric acid: sulfuric acid 1: 1.8, the flow rate ratio of setting each advection pump A, B1, B2 is m-dichlorobenzene: mixed acid: mixed acid=1: 0.7: 0.5, this time dichlorobenzene and The molar ratio of nitric acid is 1:1.2, the temperature of the first temperature zone is 10°C, the temperature of the second temperature zone is 35°C, the reaction residence time in each microchannel reactor is 30s, and the system pressure can reach 1.0Mpa. After the product comes out from the outlet, it is extracted and washed with water. According to GC analysis, the con...

Embodiment 2

[0035] (1) Device: Corning high-throughput microchannel reactor. The reactor is configured as image 3 As shown, microchannel reactor 1-4 is the first temperature zone, microchannel reactor 5-6 is the second temperature zone, and microchannel reactor 4 is supplemented with mixed acid feed. Microchannel reactor 1-2 is used for precooling mixed acid and m-dichlorobenzene.

[0036] (2) prepare mixed acid according to mass ratio nitric acid: sulfuric acid 1: 1.8, the flow rate ratio of setting each advection pump A, B1, B2 is m-dichlorobenzene: mixed acid: mixed acid=1: 0.7: 0.5, this time dichlorobenzene and The molar ratio of nitric acid is 1:1.2, the temperature of the first temperature zone is 15°C, the temperature of the second temperature zone is 30°C, the reaction residence time in each microchannel reactor is 30s, and the system pressure can reach 1.0Mpa. After the product comes out from the outlet, it is extracted and washed with water. According to GC analysis, the con...

Embodiment 3

[0038] (1) Device: Corning high-throughput microchannel reactor. The reactor is configured as image 3 As shown, microchannel reactor 1-4 is the first temperature zone, microchannel reactor 5-6 is the second temperature zone, and microchannel reactor 4 is supplemented with mixed acid feed. Microchannel reactor 1-2 is used for precooling mixed acid and m-dichlorobenzene.

[0039](2) prepare mixed acid according to mass ratio nitric acid: sulfuric acid 1: 1.8, the flow rate ratio of setting each advection pump A, B1, B2 is m-dichlorobenzene: mixed acid: mixed acid=1: 0.7: 0.5, this time dichlorobenzene and The molar ratio of nitric acid is 1:1.2, the temperature of the first temperature zone is 55°C, the temperature of the second temperature zone is 45°C, the reaction residence time in each microchannel reactor is 30s, and the system pressure can reach 1.0Mpa. After the product comes out from the outlet, it is extracted and washed with water. According to GC analysis, the conv...

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Abstract

The invention discloses a 2,4-dichloronitrobenzene synthesis method. The synthesis method is characterized in that m-dichlorobenzene and a mixed acid prepared from concentrated nitric acid and concentrated sulfuric acid are used as starting materials, and the precooling and reaction processes of the m-dichlorobenzene and the mixed acid are carried out in a high-flux micro-channel reactor. The synthesis method achieves continuous nitration reaction, and has the characteristics of high stability in temperature control and high process safety.

Description

technical field [0001] The invention relates to the nitration of aromatic hydrocarbons by using a microchannel reactor, specifically using the high-throughput microchannel reactor of Corning Corporation to synthesize 2,4-dichloronitrobenzene. Concentrated sulfuric acid mixed acid configuration, raw material pre-cooling and continuous flow process of mixed reaction. The method can continuously and safely synthesize 2,4-dichloronitrobenzene under the reaction conditions of strong mixed acid and 0-50 DEG C. Background technique [0002] 2,4-Dichloronitrobenzene is an important organic synthesis intermediate, which is widely used in chemical fields such as medicine, pesticide and dyestuff, and has broad market prospects. At present, the industrial production of 2,4-dichloronitrobenzene still adopts the traditional tank-type mechanically stirred reactor. The heat transfer rate of the reactor is very slow, and the reaction temperature needs to be strictly controlled to avoid the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/12C07C201/08
Inventor 张星邵鸿鸣
Owner ZHEJIANG YONGTAI TECH CO LTD
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