Synthesis process of 6-chloro-2, 4-dinitroaniline

A technology of dinitroaniline and synthesis process, which is applied in the preparation of amino compounds, purification/separation of amino compounds, preparation of organic compounds, etc., can solve the problems that sodium hypochlorite is not very stable, the cost of production raw materials is low, the productivity of equipment is not high, etc. Conducive to market competition, considerable economic benefits, significant effect of energy saving and emission reduction

Pending Publication Date: 2021-10-01
内蒙古融创宜博科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are significant defects in these chlorination agents and chlorination reactions, which limit their application in production
For example: (1) use sodium hypochlorite as chlorination agent, when carrying out chlorination reaction in hydrochloric acid medium, this method production process is more numerous and diverse, itself sodium hypochlorite is not very stable, and reaction process has by-product to produce, and chlorination time is longer, causes product Poor quality, dark color, low equipment productivity, and troublesome post-processing
(2) use sodium chlorate as chlorination agent, when carrying out chlorination reaction in hydrochloric acid medium, this method product purity exceeds 98%, but needs a large amount of hydrochloric acid, and contains more sodium chloride in the waste water, is unfavorable for waste water treatment, the mother liquor is less used mechanically, and the overall waste water volume is relatively large; and the raw material sodium chlorate is an explosive-produced substance, and chlorine dioxide is easily produced during the chlorination process, and chlorine dioxide is very soluble in water, which is harmful to heat, vibration, and impact. It is very sensitive to friction and easy to decompose and explode, so there are certain safety hazards
This method produces raw material cost lower, and product crystal shape is better, and color and luster is good, but chlorine gas belongs to highly toxic substance, and character is active and easily produces by-product; In addition, reaction time is long, and equipment productivity is not high, needs to regenerate acetic acid medium, Relatively large production costs need to be increased

Method used

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  • Synthesis process of 6-chloro-2, 4-dinitroaniline
  • Synthesis process of 6-chloro-2, 4-dinitroaniline
  • Synthesis process of 6-chloro-2, 4-dinitroaniline

Examples

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Embodiment 1

[0036] A kind of synthetic technique of 6-chloro-2,4-dinitroaniline, comprises the following steps:

[0037] 1) Add 150 mL of organic solvent ethyl acetate to the reaction kettle, then add 18 g of 2,4-dinitroaniline (the ratio is 8.3 L: 1 kg) to the ethyl acetate, mix well, and then add the concentration of 8 % hydrochloric acid solution 1g (the amount added is 5.56% of the mass of 2,4-dinitroaniline), stirred at 55°C for 1h to make a puree;

[0038] 2) Add 17.5g of dichlorohydantoin in batches (molar ratio: 0.9:1) to the original slurry under the condition of heat preservation at 55°C. The total time of addition is 1h, the amount of single addition is 0.875g, and the time interval is 3min. Then continue to react at 55°C for 1h;

[0039] 3) After the reaction is completed, concentrate to remove 50% of ethyl acetate, then cool to room temperature, filter, then wash the filter cake with purified water until the pH reaches 6-7, and finally dry to obtain the target product 6-chlo...

Embodiment 2

[0043]A kind of synthetic technique of 6-chloro-2,4-dinitroaniline, comprises the following steps:

[0044] 1) Add 600mL of organic solvent methanol into the reaction kettle, then add 40g of 2,4-dinitroaniline to the methanol, mix well, then add 6g of hydrochloric acid solution with a concentration of 5% to it, and stir at 45°C 1h, make puree;

[0045] 2) Add 23.6g of dichlorohydantoin in batches to the original slurry under the condition of heat preservation at 45°C, the total time of addition is 3h, the single addition amount is 1.18g, and the time interval is 9min, and then continue the reaction at 45°C 6h;

[0046] 3) After the reaction is completed, concentrate to remove 50% of methanol, then cool to room temperature, filter, then wash the filter cake with purified water until the pH reaches 6-7, and finally dry it to obtain the target product 6-chloro-2,4- Dinitroaniline 35.5g. The purity of the target product 6-chloro-2,4-dinitroaniline is ≥95.0%, and the yield is 74...

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Abstract

The present invention provides a synthesis process for 6-chloro-2, 4-dinitroaniline, which comprises: a pulping step in which 2, 4-dinitroaniline is dissolved in an organic solvent; a chlorination step in which a chlorinating agent is added to the primary pulp obtained by pulping for a reaction; and a post-treatment step after the completion of the chlorination. In the pulping step, an acid solution is also added. The chlorinating agent is 1,3-dichloro-5,5-dimethylhydantoin. According to the synthesis process, 1,3-dichloro-5,5-dimethylhydantoin is adopted as a chlorinating agent for chlorination in the liquid phase, the reaction system is stable, the material reaction is thorough, the side reaction is few, the raw material conversion rate is high, the reaction product is good in crystal form, good in color and luster, easy to separate and high in yield, the production efficiency is high, the production cost is low, the energy-saving and emission-reducing effects are remarkable, and the whole process is safe and controllable.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis process of 6-chloro-2,4-dinitroaniline. Background technique [0002] 6-chloro-2,4-dinitroaniline, also known as 2-chloro-4,6-dinitroaniline, CAS No. 3531-19-9, molecular formula C 6 h 4 ClN 3 o 4 , molecular weight 217.57, melting point 157-159°C. Easy sublimation, soluble in hot water and hot acetone, soluble in hot acetic acid. It is used as an intermediate in the production of indigo dyes and some acid dyes. As a diazo component, it is mainly used in the synthesis of disperse blue 270, 264, 259, 125 and 130 series, which can make the color of the dye itself bright and improve The colorability and fastness of dyes, the disperse dyes made from it are widely used in the printing and dyeing industry of synthetic fibers. At the same time, 6-chloro-2,4-dinitroaniline is also a fine chemical intermediate with development potential. [0003] The producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/74C07C209/84C07C209/86C07C211/52
CPCC07C209/74C07C209/84C07C209/86C07C211/52
Inventor 何卫华宋光伟周庆锋谢小强曹阳王小东
Owner 内蒙古融创宜博科技有限公司
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