Method for synthesizing 1,3-dinitrohalobenzene compound

A synthesis method and compound technology, applied in the preparation of nitro compounds, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of severe exothermic heat of nitration reaction, large content of nitric acid, high cost of waste sulfuric acid treatment, etc.
CN109970566AActive Publication Date: 2019-07-05SHANDONG HIMILE CHEM TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
SHANDONG HIMILE CHEM TECH
Publication Date
2019-07-05

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Abstract

The invention provides a method for synthesizing a 1,3-dinitrohalobenzene compound. The method comprises the following steps that A) a halogenated benzene compoundand mixed acid of nitric acid and sulfuric acid are subjected to a first nitrification reaction in a first-stage continuous flow microreactor, and oil-water separation is conducted to obtain a mononitrohalobenzene compound and first waste acid; B) the mononitrohalobenzene compound is drained into a second-stage continuous flow microreactor, a second nitrification reaction is conducted with the mixed acid of the nitric acid and the sulfuric acid, a generated nitration mixture is quenched at the outlet of the second-stage continuous flow microreactor, and filtering is conducted to obtain the 1,3-dinitrohalobenzene compound and second waste acid; C) the second waste acid is recycled to the first-stage continuous flow microreactor, a third nitration reaction with the halobenzene compound is carried out, the oil-water separation is conducted to obtain the mononitrohalobenzene compound and third waste acid, and steps B) and C) are repeated; the halobenzene compound has a structure shown in the formula I. The reaction time is short, the waste acid is less, and continuous production is achieved.
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Description

technical field

[0001] The invention relates to the technical field of chemical industry, in particular to a method for synthesizing 1,3-dinitrohalobenzene compounds. Background technique

[0002] 1,3-dinitrohalobenzene compound, its structural formula is as follows:

[0003]

[0004] R 1 is F, Cl, Br or I; R 2 For methyl, ethyl, methoxy and other electron-donating groups.

[0005] 1,3-Dinitrohalobenzene compound is an important chemical intermediate and is a useful compound in the application of hair dyes, herbicides, insecticides and dye intermediates. A common route to the synthesis of 1,3-dinitrohalobenzenes involves the nitration of halobenzenes. However, the known large-scale nitration process for 1,3-dinitrohalobenzene compounds has the following disadvantages: the reaction time is long, the mixed acid addition time of concentrated nitric acid and concentrated sulfuric acid is as long as several hours, and the amount of nitric acid is much larger. Due to the t...

Claims

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