Method for preparing 2, 4-dinitroaniline by using microreactor

A technology of dinitroaniline and microreactor, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, preparation of amino compounds, etc., can solve the problems of low production efficiency, low safety factor, high cost, and achieve High production efficiency, full equipment, full utilization effect

Pending Publication Date: 2020-09-08
杭州迈科瑞科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a method for preparing 2,4-dinitroaniline using a microreactor, which has solved the problems of low production efficiency, large pollution, high cost and safety factor of the traditional Kebai reaction. low technical issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Inject ammonia water into the preheater at a flow rate of 100ml / min, then inject 2,4-dinitrochlorobenzene into the microreactor at a rate of 926ml / min, and mix and react the two phases at 200°C for 38s to obtain product 2 , 4-dinitroaniline, after washing with water, filtering and drying, its conversion rate reaches 99.7%, and the yield is 98.6%.

Embodiment 2

[0039] Inject ammonia water into the preheater at a flow rate of 100ml / min, then inject 2,4-dinitrochlorobenzene into the microreactor at a rate of 741ml / min, and mix and react the two phases at 200°C for 41s to obtain product 2 , 4-dinitroaniline, after washing with water, filtering and drying, its conversion rate reaches 99.5%, and the yield is 98.7%.

Embodiment 3

[0041] Inject ammonia water into the preheater at a flow rate of 100ml / min, then inject 2,4-dinitrochlorobenzene into the microreactor at a rate of 556ml / min, and mix and react the two phases at 200°C for 44s to obtain product 2 , 4-dinitroaniline, after washing with water, filtering and drying, its conversion rate reaches 99.7%, and the yield is 99.1%.

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Abstract

The invention relates to the technical field of preparation of 2, 4-dinitroaniline, in particular to a method for preparing 2, 4-dinitroaniline by using a microreactor. The method comprises the following steps: (1) preparing equipment, namely preparing a preheater, the microreactor and two chromatographic pumps; (2) connecting reaction equipment, respectively connecting two chromatographic pumps with the preheater and the micro-reactor, then connecting the preheater with the micro-reactor, and putting the preheater and the microreactor into a constant-temperature oil bath after the connectionis completed; (3) conveying a reaction material, namely conveying ammonia water to the preheater at a preset flow rate, conveying the molten 2, 4-dinitrochlorobenzene to the microreactor at a preset flow rate, and mixing and reacting with the ammonia water to obtain 2, 4-dinitroaniline; and (4) after the reaction of the material in the step (3) is completed, preparing the redundant ammonia gas into ammonia water again for reuse through an ammonia gas recovery device, and continuing to reuse the ammonia generated by the reaction of ammonium chloride generated by the reaction and potassium hydroxide. Tthe method has the characteristics of high production efficiency, low energy consumption, economy, environmental protection, safety and reliability.

Description

technical field [0001] The invention relates to the technical field of 2,4-dinitroaniline preparation, and the specific field is a method for preparing 2,4-dinitroaniline by using a microreactor. Background technique [0002] Using 2,4-dinitrochlorobenzene and ammonia water as the reaction raw materials, the reaction principle of preparing 2,4-dinitroaniline is that 2,4-dinitrochlorobenzene and ammonia water undergo a bimolecular nucleophilic substitution reaction. Ammonia molecules with unshared electron pairs attack the carbon connected to the chlorine atom on the aromatic ring to obtain a polar intermediate product, which reacts rapidly and transforms into the final product 2,4-dinitroaniline. [0003] At present, the existing and previously reported production of 2,4-dinitroaniline is intermittent single-pot production and continuous-pot production, with low production efficiency, long reaction time, relatively large pollution, and high-pressure exothermic reaction. Low...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/10C07C211/52B01J19/00
CPCC07C209/10B01J19/0093B01J2219/0086C07C211/52Y02P20/10
Inventor 何强张国富周坤许英彪王康杨胡才勇谢学友赵建坤
Owner 杭州迈科瑞科技有限公司
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