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Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor

A technology of microchannel reactor and chlorophenyl nitro group, which is applied in the preparation of nitro compounds and organic chemistry, etc., to maintain the reaction temperature, avoid the phenomenon of overheating, and enhance the effect of mass transfer

Active Publication Date: 2013-12-18
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the patent and journal literature, there is no report on the continuous flow of nitric acid mixed acid configuration and the nitration of chlorobenzene mixed acid in a microchannel reactor assembled by a series of microchannel modules composed of several micro fully mixed flow structures.

Method used

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  • Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor
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  • Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Device used: Corning high-throughput microchannel reactor (Corning straight channel module + Corning heart-shaped channel module), refer to image 3 The system device diagram determines the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0034](2) Mixed acid configuration: set the mass flow rate ratio of each metering pump 1, pump 2, and pump 3 to water: nitric acid: sulfuric acid = 0.49: 0.33: 0.52, and pump them into Corning heart-shaped channel module 5 at the same time, set this section When the temperature of the heat exchanger is 30°C, the mixed acid with an effective concentration of sulfuric acid of 50% can be prepared. At this time, the molar ratio of nitric acid to sulfuric acid is 1:1.

[0035] (3) The nitric-sulfur mixed acid obtained in module 5 directly enters the mixed acid preheating module 6, a...

Embodiment 2

[0038] (1) Device used: microchannel reactor (T-shaped straight channel module + water drop channel module), refer to image 3 The system device diagram determines the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat exchange medium is water.

[0039] (2) Mixed acid configuration: set the mass flow rate ratio of each metering pump 1, pump 2, and pump 3 to water: nitric acid: sulfuric acid = 2.3: 0.33: 3.64, and pump them into the water drop channel module 5 at the same time, set this section to change When the temperature of the heater is 30°C, the mixed acid with an effective concentration of sulfuric acid of 60% can be prepared. At this time, the molar ratio of nitric acid to sulfuric acid is 1:7.

[0040] (3) The nitric-sulfur mixed acid obtained in module 5 directly enters the preheating module 6, and the preheating and reaction temperature are set to 60°C, ...

Embodiment 3

[0043] (1) The device used: microchannel reactor (T-shaped straight channel module + spherical baffle-type channel module), and the heat exchange medium is heat transfer oil. refer to image 3 The system device diagram determines the connection mode of the microchannel reactor, and the number of mixed reaction modules is determined according to the flow rate and reaction residence time.

[0044] (2) Mixed acid configuration: set the mass flow rate ratio of each metering pump 1, pump 2, and pump 3 to water: nitric acid: sulfuric acid = 1.03: 0.33: 2.6, and pump them into the ball-shaped baffle-shaped channel module 5 at the same time, set Set the temperature of the heat exchanger in this section as 30°C, and the mixed acid with an effective concentration of sulfuric acid of 70% can be configured. At this time, the molar ratio of nitric acid to sulfuric acid is 1:5.

[0045] (3) The nitric-sulfur mixed acid obtained in module 5 directly enters the mixed acid preheating module ...

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Abstract

The invention relates to a method for undergoing a chlorobenzene nitration reaction by using a micro-channel reactor, belonging to the technical field of application of organic synthesis. In the method, nitric acid, sulfuric acid, water and chlorobenzene are taken as initial reaction raw materials, and processes such as mixed acid preparation, mixed acid and chlorobenzene preheating, mixed acid and chlorobenzene reacting and the like are completed in a micro-channel reactor system. In the reaction, nitro-sulfuric mixed acid is taken as a nitrating agent, the effective concentration of sulfuric acid in the mixed acid is 50-90 percent, the molar ratio of the nitric acid to the sulfuric acid in the mixed acid is 1:1-1:10, the molar ratio of the chlorobenzene to the nitric acid is 1:1.0-1:2.0, the reaction temperature is 50-100 DEG C, and the reaction time is 30-120 seconds. The chlorobenzene transformation ratio is up to 97 percent, the selectivity of nitrochlorobenzene serving as a product is over 96.5 percent, and the ratio of ortho-para nitrochlorobenzene is over 0.6. A strengthened mixed micro-channel reactor adopted in the invention is particularly suitable for undergoing a continuous nitration reaction, and has the characteristics of stable temperature control and safe process.

Description

technical field [0001] The present invention relates to utilizing microchannel reactor to carry out aromatic hydrocarbon nitration, and specific content comprises utilizing the channel module that is made up of multiple miniature fully mixed flow structural units to be combined into enhanced mixing type microchannel reactor (such as Corning Inc. Corning's high-throughput microchannel Reactor), the method for synthesizing nitrochlorobenzene by using the reactor is a continuous flow process in which the nitrating agent, nitric acid and sulfur mixed acid are configured, the raw materials are preheated, and the nitration reaction process is completed in a microchannel reactor. The method can continuously and safely synthesize nitrochlorobenzene under the reaction conditions of strong mixed acid and 50-100 DEG C. technical background [0002] Microchannel reactors generally refer to small reaction systems manufactured through micro-processing and precision processing technologies...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/12C07C201/08
Inventor 严生虎张跃张沫刘建武沈介发马兵沈卫姜冬明
Owner CHANGZHOU UNIV
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