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Production method of 2,4-dinitraniline

A technology of dinitroaniline and its production method, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of low production cost, high energy consumption, high production safety risk, etc., and achieve low production cost , control the reaction rate, and reduce the production safety risk

Inactive Publication Date: 2017-11-24
浙江大井化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a low-temperature and low-pressure production method for 2,4-dinitroaniline to solve the problems of high production safety risk and high energy consumption in the prior art. Reduce the safety risk of production, with the characteristics of high product yield, good product quality and low production cost

Method used

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  • Production method of 2,4-dinitraniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 980L of water to the reaction kettle, raise the temperature to 62°C, add 1180Kg 2,4-dinitrochlorobenzene, raise the temperature to 82°C again, add 1475Kg of ammonia water with a concentration of 18wt% dropwise at a uniform speed, and control the temperature at 83-85°C. The pressure is controlled at 0.05MPa, and the dropping time is 4 hours and 10 minutes. After the dropping is completed, the temperature is raised to 95°C, the pressure is at 0.09MPa, and the reaction is kept for 2 hours. The end point is detected by liquid chromatography. That is, a light yellow powdery 2,4-dinitroaniline product was obtained, with a product purity of 99.52% and a product yield of 99.12%. After the product was dried, the fineness of the product was 20-40 mesh, accounting for 95.3% by mass.

Embodiment 2

[0025] Add 1063L of water to the reactor, heat up to 65°C, add 1250Kg of 2,4-dinitrochlorobenzene, heat up to 81°C again, add 1587Kg of ammonia water with a concentration of 18wt% dropwise at a constant speed, and control the temperature at 81-84°C. The pressure is controlled at 0.06MPa, and the dropping time is 4 hours and 05 minutes. After the dropping is completed, the temperature is raised to 96°C, the pressure is at 0.10MPa, and the reaction is kept for 2 hours. The end point is detected by liquid chromatography. That is, the light yellow powdery 2,4-dinitroaniline product is obtained, the product purity is 99.43%, and the product yield is 99.21%. After the product is dried, the fineness of the product is 20-40 mesh, accounting for 92.1% by mass.

Embodiment 3

[0027] Add 985L of water to the reaction kettle, raise the temperature to 63°C, add 1200Kg of 2,4-dinitrochlorobenzene, raise the temperature to 80°C again, add 1475Kg of ammonia water with a concentration of 18wt% dropwise at a uniform speed, and control the temperature at 81-85°C. The pressure is controlled at 0.05MPa, and the dropping time is 3 hours and 55 minutes. After the dropping is completed, the temperature is raised to 92°C, the pressure is at 0.10MPa, and the reaction is kept for 2 hours. The end point is detected by liquid chromatography. The light yellow powdery 2,4-dinitroaniline product was obtained, the product purity was 99.23%, and the product yield was 99.06%. After the product was dried, the fineness of the product was 20-40 mesh, accounting for 90.4% by mass.

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Abstract

The invention discloses a production method of 2,4-dinitraniline. 2,4-dinitrochlorobenzene and ammonium hydroxide are taken as raw materials; the method comprises steps as follows: bottom water is added to a reaction kettle, heated to 50-70 DEG C, mixed with 2,4-dinitrochlorobenzene and then heated, ammonium hydroxide is dropwise added, the mixture is heated to 90-100 DEG C after addition, the pressure is controlled at 0.05-0.1 MPa, the thermal insulation reaction is performed for 1-3 hours, and 2,4-dinitraniline is obtained through centrifugal filtration. 2,4-dinitraniline is produced with a low-temperature and low-pressure method, the reaction conditions are mild, the production safety risk is low, a high-quality product is obtained through centrifugal filtration after the reaction ends, further purification and separation are not required, and the production cost is low.

Description

technical field [0001] The invention relates to the production of dye intermediates, in particular to a production method of 2,4-dinitroaniline. Background technique [0002] 2,4-Dinitroaniline is an intermediate of disperse dyes, neutral dyes, sulfur dyes and organic pigments. Used in the production of sulfur dark blue 3R, disperse red B, disperse violet 2R and other dyes. It is also used in other organic synthesis, the production of pesticide dinitrate powder, etc., as well as the toner of printing ink and the preparation of preservatives. [0003] The existing production method of 2,4-dinitroaniline is to take 2,4-dinitrobenzene chloride as raw material, add 18wt% ammonia water at one time and carry out ammonolysis reaction, the ammonolysis pressure is 0.48MPa, and the ammonolysis temperature is 140-150°C, the ammonolysis time is about 2 hours. The disadvantages of this process are high production safety risks, high energy consumption, serious material accumulation in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/10C07C211/52
CPCC07C209/10C07C211/52
Inventor 杨尧森阮海良邱玉成夏骏钢
Owner 浙江大井化工有限公司
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