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A kind of method utilizing microchannel reactor to synthesize 2,4-dichloro-3-fluoronitrobenzene

A microchannel reactor and fluoronitrobenzene technology are applied in the field of aromatic hydrocarbon nitration to achieve the effects of improving conversion rate, ensuring safety and improving selectivity

Active Publication Date: 2016-04-13
ZHEJIANG YONGTAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The nitration of 2,6-dichlorofluorobenzene to synthesize 2,4-dichloro-3-fluoronitrobenzene using a microchannel reactor has not been reported in the literature

Method used

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  • A kind of method utilizing microchannel reactor to synthesize 2,4-dichloro-3-fluoronitrobenzene
  • A kind of method utilizing microchannel reactor to synthesize 2,4-dichloro-3-fluoronitrobenzene
  • A kind of method utilizing microchannel reactor to synthesize 2,4-dichloro-3-fluoronitrobenzene

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Experimental program
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Effect test

Embodiment 1

[0028] (1) Device: Corning high-throughput microchannel reactor, model G1. like figure 1 As shown, the microchannel reactor 1-3 is a heart-shaped structure.

[0029] (2) The mixed acid is prepared according to the mass ratio of nitric acid: sulfuric acid 1:2.53, 2,6-dichlorofluorobenzene is dissolved by adding 20% ​​dichloromethane, and the advection pump A is used to feed 2,6-dichlorofluorobenzene, and the flow rate is set is 50ml / min, which is equivalent to 0.35mol / min of 2,6-dichlorofluorobenzene. The molar ratio of dichlorofluorobenzene to nitric acid is 1:1, mixed acid and 2,6-dichlorofluorobenzene are reacted in microchannel reactors 1-3, the reaction temperature is 40°C, and each microchannel reactor The reaction residence time is 15s, and the system pressure is 0.6Mpa. After the product comes out of the outlet, it is extracted and washed with water. According to GC analysis, the conversion rate of 2,6-dichlorofluorobenzene is 88%, and the selectivity of 2,4-dichloro...

Embodiment 2

[0031] (1) Device: Corning high-throughput microchannel reactor, model G1. like figure 1 As shown, the microchannel reactor 1-3 is a heart-shaped structure.

[0032] (2) The mixed acid is prepared according to the mass ratio of nitric acid: sulfuric acid 1:2.53, 2,6-dichlorofluorobenzene is dissolved by adding 20% ​​dichloromethane, and the advection pump A is used to feed 2,6-dichlorofluorobenzene, and the flow rate is set is 50ml / min, which is equivalent to 0.35mol / min of 2,6-dichlorofluorobenzene. The molar ratio of dichlorofluorobenzene to nitric acid is 1:1, mixed acid and 2,6-dichlorofluorobenzene are reacted in microchannel reactors 1-3, the reaction temperature is 40°C, and each microchannel reactor The reaction residence time is 15s, and the system pressure is 1Mpa. After the product comes out of the outlet, it is extracted and washed with water. According to GC analysis, the conversion rate of 2,6-dichlorofluorobenzene is 79%, and the selectivity of 2,4-dichloro-3...

Embodiment 3

[0034] (1) Device: Corning high-throughput microchannel reactor, model G1. like figure 1 As shown, the microchannel reactor 1-3 is a heart-shaped structure.

[0035] (2) The mixed acid is prepared according to the mass ratio of nitric acid: sulfuric acid 1:2.53, 2,6-dichlorofluorobenzene is dissolved by adding 20% ​​dichloromethane, and the advection pump A is used to feed 2,6-dichlorofluorobenzene, and the flow rate is set is 50ml / min, which is equivalent to 0.35mol / min of 2,6-dichlorofluorobenzene. The molar ratio of dichlorofluorobenzene to nitric acid is 1:1, mixed acid and 2,6-dichlorofluorobenzene are reacted in microchannel reactors 1-3, the reaction temperature is 40°C, and each microchannel reactor The reaction residence time is 15s, and the system pressure is 0.5Mpa. After the product comes out of the outlet, it is extracted and washed with water. According to GC analysis, the conversion rate of 2,6-dichlorofluorobenzene is 80%, and the selectivity of 2,4-dichloro...

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Abstract

The invention discloses a method for synthesizing 2, 4-dichloro-3-fluoronitrobenzene by means of micro-channel reactors. The process that 2, 6- dichlor fluorbenzene reacts with mixed acid is completed in the high-flux micro-channel reactors, a continuous nitration reaction can be conducted, and the method has the advantages that temperature control is stable and the process is safe.

Description

technical field [0001] The invention relates to the nitration of aromatic hydrocarbons using a microchannel reactor, specifically a method for synthesizing 2,4-dichloro-3-fluoronitrobenzene by using a high-throughput microchannel reactor of Corning Corporation, which is a method in a microchannel reactor Complete the continuous flow process of concentrated nitric acid and concentrated sulfuric acid mixed acid configuration and mixed reaction. The method can continuously and safely synthesize 2,4-dichloro-3-fluoronitrobenzene under the reaction conditions of strong mixed acid and 20-100 DEG C. Background technique [0002] 2,4-Dichloro-3-fluoronitrobenzene is a key intermediate of quinolones. At present, the industrial production of 2,4-dichloro-3-fluoronitrobenzene still adopts the traditional tank-type mechanically stirred reactor. The efficiency is low, and the unavoidable uneven mixing of materials by ordinary stirring leads to low conversion rate of raw materials and h...

Claims

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Application Information

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