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
CN102432471BActive Publication Date: 2013-12-18CHANGZHOU UNIV

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
CHANGZHOU UNIV
Publication Date
2013-12-18

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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.
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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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