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Preparation method of 2,4-binitro-6-chloroaniline

A technology of dinitroaniline and chloroaniline, which is applied in the chemical industry, can solve the problems of high local reaction temperature, difficulty in control, and easy explosion of chlorine dioxide, and achieve the effect of improving product quality and yield

Active Publication Date: 2014-08-27
浙江汇翔新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The local reaction temperature is high, it is difficult to control, and it is easy to produce polychlorinated compounds;
[0006] 2. Since the generated chlorine gas and sodium chlorate have many contact opportunities, the generated chlorine dioxide is easy to explode, and there are serious safety hazards;
[0007] 3. The quality of the product is poor, the HPLC purity is 94-95%, and the residue of 2,4-dinitroaniline is about 4%;
[0008] 4. The energy consumption is high, and a large amount of circulating water is required to control the temperature;
[0010] 6. Too much sodium chlorate produces a lot of waste gas

Method used

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  • Preparation method of 2,4-binitro-6-chloroaniline
  • Preparation method of 2,4-binitro-6-chloroaniline
  • Preparation method of 2,4-binitro-6-chloroaniline

Examples

Experimental program
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Effect test

Embodiment 1

[0042] 611.8kg of 2,4-dinitroaniline, 400kg of water, dispersed to 20±5μm by dispersion pump, added to 1050kg of 30-35% hydrochloric acid, heated to 70°C, stirred at 70-75°C for 1-2 hours, cooled to 50-60°C for use.

[0043] Dissolve 120kg of sodium perchlorate in 250kg of water to make a sodium chlorate solution below 40°C for use.

[0044] 412kg of 2,4-dinitroaniline solution per hour and 74kg of sodium chlorate solution per hour enter the pipeline reactor at the same time. The total residence time in the pipeline reactor is 3-10 seconds. Hours, when the end point is reached, it is centrifuged and dried, air-dried, the mother liquor is treated and recycled, and dried to obtain 710-720kg of 2.4-dinitro-6-chloroaniline with a water content of ≤2% and a yield of about 98%.

Embodiment 2

[0046] The weight of 2,4-dinitroaniline is 611.8kg, and the mother liquid water containing 15% hydrochloric acid is 2100kg. After beating evenly, the dispersion pump is dispersed to 20±5μm for use.

[0047] 120kg of sodium perchlorate and 300kg of water are used to make a sodium chlorate solution below 40°C for use.

[0048] Use a metering pump to preheat 500kg of 2,4-dinitroaniline liquid per hour to 50-60°C through the preheater, and enter the pipeline reactor. At the same time, the metering pump injects 84kg of sodium chlorate into the pipeline for reaction In the pipeline reactor, the continuous reaction residence time of the pipeline reactor is 3-10 seconds, enter the aging tank and keep at 70±10°C for 2 hours, central control, centrifuge, and dry to obtain 2.4-dinitro -6-chloroaniline 715kg.

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Abstract

The invention relates to the chemical industry field, in particular relates to a preparation method of 2,4-binitro-6-chloroaniline. The preparation method of the 2,4-binitro-6-chloroaniline is carried out under heat insulation condition by adopting a pipeline reactor, the process from contact of the materials to reaction is finished instantly without producing polychlorinated compounds and chlorine dioxide, the potential safety hazard is avoided, the product quality and yield are greatly improved, the HPLC (high performance liquid chromatography) purity is not less than 98%, and the 2,4-dinitraniline residue is not more than 1%; the final product does not come into contact with oxidized sodium chlorate and chlorine due to adoption of the pipeline continuous reaction, no oxidation product is produced in the system, the product quality is improved, and the infinite recycling of the master liquid can be realized; the mother liquid is filtered through a film to recycle sodium chloride, and the infinite recycling of the mother liquid is realized after the mother liquid adsorbs hydrogen chloride, and the sodium chlorate approaches to a theoretical consumption.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of 2,4-dinitro-6-chloroaniline. Background technique [0002] The existing technology is to add 2.4-dinitroaniline, hydrochloric acid, water in the reactor, and drop sodium chlorate under the liquid, and the reaction equation is: [0003] [0004] Its disadvantages are: [0005] 1. The local reaction temperature is high, it is difficult to control, and it is easy to produce polychlorinated compounds; [0006] 2. Because the chlorine gas and sodium chlorate have many contact opportunities, the chlorine dioxide produced is easy to explode, and there are serious safety hazards; [0007] 3. The quality of the product is poor, the HPLC purity is 94-95%, and the residue of 2,4-dinitroaniline is about 4%; [0008] 4. The energy consumption is high, and a large amount of circulating water is required to control the temperature; [0009] 5. The reaction concent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/74
Inventor 段玉辉沈林峰
Owner 浙江汇翔新材料科技股份有限公司
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