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A kind of synthetic technique of 2,4-dinitro-6-chloroaniline

A technology of dinitroaniline and synthesis process, which is applied in the preparation of amino compounds, the preparation of organic compounds, organic chemistry, etc. It can solve the problems of high acid content in mother liquor wastewater, fewer batches of mother liquor that can be recycled, and increased wastewater discharge. , achieve significant energy saving and emission reduction, reduce waste water discharge, and use less acid

Active Publication Date: 2018-05-11
ZHEJIANG LONGSHENG GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the concentration of hydrochloric acid used in this patent is high, the cost is high, and the mother liquor can be circulated in a small number of batches, the acid content of the mother liquor wastewater is high, and the acid content in the filter cake is also high, and the water consumption is large during washing, which also increases the waste water. emissions

Method used

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  • A kind of synthetic technique of 2,4-dinitro-6-chloroaniline
  • A kind of synthetic technique of 2,4-dinitro-6-chloroaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 350 g of 5% hydrochloric acid and 0.4 g of 4-dimethylaminopyridine into a 500 ml three-necked flask with a stirrer and a thermometer, and stir for 15 min; after the stirring time is up, add finely ground 2,4-dinitroaniline 73.2 g, after beating at 25°C for 1 hour, slowly introduce 14.2g of chlorine gas, the time of chlorine gas flow is controlled at 2-3 hours, the temperature of chlorine flow is controlled at 30-35°C, after the chlorine gas is passed, the temperature is raised to 55°C and 27% of Sodium chlorate solution 34.18g, dropwise time is 1h, reaction temperature is controlled at 55~60°C, keep warm for 2h after dropwise addition, then filter, filter cake is washed with 2% liquid caustic to neutrality, obtains 6-chloro- 2,4-dinitroaniline, purity 97.5%, yield 95.6%, mother liquor is collected and applied mechanically to the next batch of reactions, according to the above steps, when the mother liquor is continuously applied mechanically for 15 batches, the conce...

Embodiment 2

[0030] Add 350g of 6% hydrochloric acid and 0.4g of sodium dodecylbenzenesulfonate into a 500ml three-necked flask with a stirrer and a thermometer, and stir for 15 minutes; after the stirring time is up, add finely ground 2,4-dinitro 73.2g of aniline, after beating at 25°C for 1 hour, slowly feed 11.36g of chlorine gas, the time of chlorine gas flow is controlled at 2-3 hours, the temperature of chlorine flow is controlled at 35-40°C, after the completion of chlorine gas flow, the temperature is raised to 50°C, and 27 % sodium chlorate solution 39.96g, the time for dropping is 1h, the reaction temperature is controlled at 50~55°C, after the dropwise addition is completed, it is incubated for 2h, then filtered, and the filter cake is washed to neutrality with 2% liquid alkali to obtain 6- Chloro-2,4-dinitroaniline, the purity is 96.5%, the yield is 95.8%. The mother liquor is collected and applied to the next batch of reactions. According to the above steps, when the mother liq...

Embodiment 3

[0032] Add 350g of 3% hydrochloric acid and 0.4g of dispersant MF into a 500ml three-neck flask equipped with a stirrer and a thermometer, and stir for 15min; after the stirring time is up, add 54.9g of 2,4-dinitroaniline. After beating at 30°C for 1 hour, slowly feed 12.78g of chlorine gas, the time of chlorine gas flow is controlled at 2-3 hours, the temperature of chlorine gas flow is controlled at 30-35°C, after the chlorine gas is passed, the temperature is raised to 55°C and the concentration of mass percentage is 27. % sodium chlorate solution 20.19g, the dropping time is 1h, and the reaction temperature is controlled at 55-60°C. After the dropping is completed, keep warm for 2h, then filter, and wash the filter cake with water until neutral to obtain 6-chloro-2,4 -Dinitroaniline, purity 96.3%, yield 96.0%, mother liquor is collected and applied mechanically to the next batch of reactions, according to the above steps, when mother liquor is continuously applied mechanica...

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Abstract

A synthetic technology for 2-chloro-4,6-dinitroaniline is disclosed. The technology comprises (1) dispersing 2,4-dinitroaniline in hydrochloric acid and a catalyst and stirring to form a slurry, wherein the mass fraction of hydrochloric acid is 1-8%; (2) introducing chlorine into the slurry obtained in the step (1) for chlorination reaction; (3) adding a sodium chlorate solution into the reaction solution in the step (2) and continuing performing chlorination reaction, wherein the mass fraction of the sodium chlorate solution is 20%-40%; and (4) filtering the reaction solution obtained in the step (3), washing the filter cake until the pH value is 6.0-7.0, returning the mother liquid to the step (1) as hydrochloric acid and the catalyst for cyclic utilization utile the sodium chloride in the mother liquid is saturated, and discharging the mother liquid into a wastewater processing system, wherein the molar ratio of 2,4-dinitroaniline, chlorine and sodium chlorate is 1:(0.2-0.8):(0.06-0.3). The technology is high in yield, the purity of the obtained product is high, cost is low, the cycling times of the mother liquid are more, the wastewater discharging amount is less, and the benifit of energy saving and emission reduction is substantial.

Description

(1) Technical field [0001] The invention relates to a synthesis process of 2,4-dinitro-6-chloroaniline. (2) Background technology [0002] 2,4-Dinitro-6-chloroaniline is an important intermediate of disperse dyes, and it is widely used both at home and abroad. Its production method is generally obtained by chlorination of 2,4-dinitroaniline as raw material. Chlorinating agents mainly include: (1) sodium hypochlorite; (2) sodium chlorate; (3) chlorine gas. [0003] (1) Use sodium hypochlorite as the chlorination agent to carry out chlorination reaction in hydrochloric acid medium. The production process of this method is more complicated, and by-products are produced in the reaction process, the product quality is poor, the color is deep, the chlorination time is long, and the equipment productivity is low , and the post-processing is more troublesome. [0004] (2) use sodium chlorate as chlorination agent, carry out chlorination reaction in hydrochloric acid medium, this ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/52C07C209/74
Inventor 余青结祝培明张友珍曾银城李世华郭塬智倪松涛李君韩伟
Owner ZHEJIANG LONGSHENG GROUP
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