Clean production process of 6-chloro-2,4-dinitroaniline

A dinitroaniline, clean production technology, applied in the preparation of amino compounds, the preparation of organic compounds, organic chemistry and other directions, can solve the problems of long chlorination time, troublesome post-processing, low equipment productivity, etc., and achieves fast reaction speed, Less side effects

Active Publication Date: 2014-01-29
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

[0016] The method uses sodium hypochlorite as the chlorination agent, and many by-products are produced in the reaction process, the product

Method used

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  • Clean production process of 6-chloro-2,4-dinitroaniline
  • Clean production process of 6-chloro-2,4-dinitroaniline
  • Clean production process of 6-chloro-2,4-dinitroaniline

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0036] Example 1

[0037] In a 500 ml flask with a stirrer and a thermometer, 350 g of hydrochloric acid with a mass percentage concentration of 12% was added, and 54.9 g of 2,4-dinitroaniline was added. After beating at 20°C for half an hour, slowly pass in 10.65g of chlorine gas, the time of passing chlorine is 2 hours, and the temperature of passing chlorine is 20-40°C. After heating for half an hour, the temperature is slowly raised to 40°C, and 30% mass percentage concentration is added dropwise. The sodium chlorate solution is 21.3g, the dropping time is 1 hour, and the reaction temperature is 40-55°C. After dripping and keeping for half an hour, filtering and washing with water yield 6-chloro-2,4-dinitroaniline with a purity of 98.4% and a yield of 96.5%. The mother liquor is collected and used in the next batch. The mother liquor was continuously used in 10 batches, with an average purity of 97.2% and a yield of 96.9%.

Example Embodiment

[0038] Example 2

[0039] In a 500 ml flask with a stirrer and a thermometer, 350 g of hydrochloric acid with a concentration of 18% by mass is added, and 54.9 g of 2,4-dinitroaniline is added. After beating at 30°C for half an hour, slowly pass in 6.39g of chlorine gas, the time of passing chlorine is 1 hour, and the temperature of passing chlorine is 20-40°C. After heating for half an hour, the temperature is slowly raised to 40°C, and 30% sodium chlorate solution is added dropwise. 29.8g, the dropping time is 1.5 hours, and the reaction temperature is 40-55°C. After dripping and keeping it for half an hour, filtering and washing with water yield 6-chloro-2,4-dinitroaniline with a purity of 97.8% and a yield of 96.2%. The mother liquor is collected and used in the next batch. The mother liquor was continuously used in 10 batches, with an average purity of 96.8% and a yield of 96.5%.

Example Embodiment

[0040] Example 3

[0041] Add 490 g of hydrochloric acid with a concentration of 15% by mass in a 1000 ml flask with a stirrer and a thermometer, and add 54.9 g of 2,4-dinitroaniline. After beating at 30°C for half an hour, slowly pass 8.52g of chlorine gas, the time of passing chlorine is 2 hours, and the temperature of passing chlorine is 20-40°C. After heating for half an hour, the temperature is slowly raised to 40°C, and 30% sodium chlorate solution is added dropwise. 25.56g, the dropping time is 1.5 hours, and the reaction temperature is 40-55°C. After dripping for half an hour, filtering and washing with water to obtain 6-chloro-2,4-dinitroaniline with a purity of 98.5% and a yield of 96.1%. The mother liquor is collected and used in the next batch. The mother liquor was continuously used in 10 batches, with an average purity of 97.1% and a yield of 95.8%.

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Abstract

The invention discloses a clean production process of 6-chloro-2,4-dinitroaniline. The clean production process of 6-chloro-2,4-dinitroaniline comprises the following steps: 1, dispersing 2,4-dinitroaniline into hydrochloric acid solution for pulping, then introducing chlorine gas into the solution for reacting, and thus obtaining intermediate reaction solution; and 2, adding the intermediate reaction solution obtained in the step 1 into sodium chlorate solution for reacting, after the reaction is completed, processing the reaction solution to obtain the 6-chloro-2,4-dinitroaniline and mother solution, and returning the mother solution to the step 1 to serve as the hydrochloric acid solution. According to the production process, the chlorine gas and the sodium chlorate are sequentially employed as chloride agents for chlorinating in steps, so that the product purity and yield are improved and the cost of material is reduced; and the quantity of hydrochloric acid after the reaction is completed is kept stable basically, so that the mother solution is convenient to recycle for use and the pollution to environment is reduced.

Description

technical field [0001] The invention belongs to the field of synthesis of dye intermediates, in particular to a clean production process for 6-chloro-2,4-dinitroaniline. Background technique [0002] 6-Chloro-2,4-dinitroaniline, also known as 2-chloro-4,6-dinitroaniline, has the structure shown in formula (I), and its CAS number is 3531-19-9. It is an important Dye intermediates, as diazo components, are mainly used in the synthesis of disperse blue 270, 264, 259, 125 and 130, etc., and the disperse dyes made from it are widely used in the printing and dyeing industry of synthetic fibers. [0003] [0004] At present, there are four main synthetic methods of 6-chloro-2,4-dinitroaniline, which are introduced as follows: [0005] (1) 2,4-Dinitroaniline is beaten in hydrochloric acid, and the sodium chlorate prepared as a solution is slowly added to the beating material for chlorination reaction to obtain the product. The reaction formula is as follows: [0006] [000...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/74
Inventor 陈宝兴赵国生阮海兴高立江
Owner 浙江大井化工有限公司
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