Method for synthesizing nitryl chloroaniline compound by using micro-channel reactor

A micro-channel reactor, the technology of nitrochloroaniline is applied in the field of nitration of chloroaniline, and achieves the effects of rapid and uniform mixing, maintaining the reaction temperature, and reducing the generation of by-products

Inactive Publication Date: 2013-05-22
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in patents and periodical literature, there is no report of continuous flow of chloroanilide acylation and nitration in a microchannel reactor.

Method used

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  • Method for synthesizing nitryl chloroaniline compound by using micro-channel reactor
  • Method for synthesizing nitryl chloroaniline compound by using micro-channel reactor
  • Method for synthesizing nitryl chloroaniline compound by using micro-channel reactor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) The device used: microchannel reactor, and the heat transfer medium is heat transfer oil.

[0034] (2) Refer to image 3Determine the connection mode of the microchannel reactor. The reaction residence time is determined according to the length and flow rate of the straight channel. The circulating heat transfer oil is used as the heat exchange medium, and the reaction temperature is set at 50°C. The molar flow rate ratio of each metering pump is p-chloroaniline:acyl chloride:nitric acid:sulfuric acid=1:1.4:1:0.05, the reaction residence time is 40s, and the reaction product flows out of the reactor and enters the lye hydrolysis tank reactor. The product can be detected by liquid chromatography through extraction, neutralization and washing. At this moment, the conversion rate of p-chloroaniline is 100%, and the mass content of acylated chloroaniline is 5.5% in the product, and the mass content of 5-nitro-p-chloroaniline is 92%.

Embodiment 2

[0036] (1) The device used: microchannel reactor, and the heat exchange medium is water.

[0037] (2) Refer to image 3 Determine the connection mode of the microchannel reactor. The reaction residence time is determined according to the length and flow rate of the straight channel. The circulating heat transfer oil is used as the heat exchange medium, and the reaction temperature is set at 70°C. The molar flow rate ratio of each metering pump is o-chloroaniline: acid anhydride: nitric acid: sulfuric acid = 1: 1.6: 1.1: 0.07, the reaction residence time is 60s, and the reaction product flows out of the reactor and enters the lye hydrolysis tank reactor. The product can be detected by liquid chromatography after extraction, neutralization and washing. At this time, the conversion rate of o-chloroaniline is 100%, the mass content of acylated chloroaniline in the product is 7.5%, and the content of 4-nitro-p-chloroaniline is 64.3% %, the mass content of 3-nitro-p-chloroaniline i...

Embodiment 3

[0039] (1) The device used: microchannel reactor, and the heat exchange medium is water.

[0040] (2) Refer to image 3 Determine the connection mode of the microchannel reactor. The reaction residence time is determined according to the length and flow rate of the straight channel. The circulating heat transfer oil is used as the heat exchange medium, and the reaction temperature is set at 90°C. The molar flow rate ratio of each metering pump is m-chloroaniline: glacial acetic acid: nitric acid: sulfuric acid = 1: 1.8: 1.2: 0.09, the reaction residence time is 80s, and the reaction product flows out of the reactor and enters the lye hydrolysis tank reactor. The product can be detected by liquid chromatography through extraction, neutralization and washing. At this moment, the m-chloroaniline conversion rate is 100%, and the acylated chloroaniline mass content is 2.3% in the product, and the 2-nitro-m-chloroaniline mass content is 20.7%, and the mass content of 4-nitro-m-chlo...

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Abstract

The invention relates to a method for synthesizing nitryl chloroaniline compound by using a micro-channel reactor, and belongs to the technical field of organic synthesis application. In the method, chloroaniline, acylating agent, nitric acid and sulfuric acid are used as original reaction raw materials, the processes of chloroaniline acylation, mixture acid confection, acylated chloroaniline nitration, and the like are carried out in the micro-channel reactor system, and a hydrolysis reaction process is finished out of the micro-channel device by using a normal reactor. In the reaction, acyl chloride, acid anhydride and glacial acetic acid are used as the acylating agent, and nitric acid and sulfuric acid mixture acid is used as the nitrating agent, the chloroaniline acylation transformation rate can reach 100%, and the mass content of the nitryl chloroaniline reaches higher than 92%. The micro-channel reactor used in the invention is especially suitable for carrying out continuously acylation and nitration reaction, and has the characteristics of being stable in temperature control and safe in process.

Description

technical field [0001] The invention relates to the nitration of chloroaniline by using a microchannel reactor, and the specific content includes the method of using the reactor to protect and nitrate the amino groups of chloroaniline and the hydrolysis reaction outside the reactor. Thermal, amine protection, continuous flow process for nitration reaction process. The method can continuously and safely synthesize nitrochlorobenzene under the reaction conditions of strong mixed acid and 50-110 DEG C. technical background [0002] Microchannel reactors generally refer to small reaction systems manufactured through micro-processing and precision processing technologies. It includes mixers, heat exchangers, reactors, controllers, etc. required by chemical units, but its pipe size is much smaller than that of conventional tubular reactors, and its miniaturized structure makes it have some new features. [0003] The nitration of chloroaniline is an important chemical industry re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/76
Inventor 张跃张沫严生虎刘建武沈介发马兵沈卫
Owner CHANGZHOU UNIV
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