Method for preparing ortho-nitroaniline by high pressure ammonolysis

A technology for o-nitroaniline and o-chloronitrobenzene, applied in the field of preparing o-nitroaniline, can solve the problems of complex production operation, many reaction steps, few industrialized production and the like, and achieves low production cost, simple operation, good quality The effect of industrial application prospects

Inactive Publication Date: 2014-06-18
凯美泰克(天津)化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has many reaction steps and complex production operations, and is rarely used in industrial production.

Method used

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  • Method for preparing ortho-nitroaniline by high pressure ammonolysis

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Experimental program
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Effect test

Embodiment 1

[0022] Add 800g of o-chloronitrobenzene and 300g of liquid ammonia to a 2L autoclave, raise the temperature to 170°C, press at 8MPa, keep at 170°C for 7 hours, cool down, recover excess liquid ammonia, then add 1000g of toluene into the reaction kettle, and stir for 15 Minutes later, it was filtered, and the obtained filtrate was distilled to recover the solvent to obtain 681 g of o-nitroaniline with a gas chromatography purity of 99.5% and a molar yield of 97.1%.

Embodiment 2

[0024] Add 800g of o-chloronitrobenzene and 480g of liquid ammonia to a 2L autoclave, raise the temperature to 150°C, press at 10MPa, keep at 150°C for 15 hours, cool down, recover excess liquid ammonia, and then add 1000g of dichloroethane into the reaction kettle , after stirring for 15 minutes, filtered, and the obtained filtrate was distilled to recover the solvent to obtain 683g of o-nitroaniline, with a gas chromatography purity of 99.6% and a molar yield of 97.4%.

Embodiment 3

[0026] Add 800g of o-chloronitrobenzene and 240g of liquid ammonia to a 2L autoclave, raise the temperature to 200°C, and the pressure is 7.5MPa, keep at 200°C for 11 hours, cool down, recover excess liquid ammonia, then add 1000g of toluene into the reaction kettle, stir After 15 minutes, it was filtered, and the obtained filtrate was distilled to recover the solvent to obtain 675 g of o-nitroaniline with a gas chromatography purity of 99.2% and a molar yield of 96.2%.

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Abstract

The invention discloses a method for preparing ortho-nitroaniline by high pressure ammonolysis. The method comprises the following steps: enabling o-chloronitrobenzene and liquid ammonia to generate an ammonolysis reaction under the high pressure to generate a reaction mixture containing o-chloronitrobenzene, unreacted liquid ammonia and ammonium chloride which is a byproduct, recycling the unreacted liquid ammonia from the reaction mixture, then adding a solvent to the rest reaction mixture, removing ammonium chloride solid through filtering, and removing the solvent from filtrate to obtain the ortho-nitroaniline, wherein the high pressure (gauge pressure) is 6-10MPa. According to the method disclosed by the invention, the problem that a great deal of wastewater containing ammonium chloride, which is difficult to treat, is generated in the traditional process is solved. Therefore, the method disclosed by the invention is low in production cost, simple to operate, free of generation of wastewater and environment-friendly and has a favorable industrial application prospect.

Description

technical field [0001] The invention relates to a method for preparing o-nitroaniline by high-pressure ammonolysis of o-chloronitrobenzene. Background technique [0002] O-nitroaniline is an important intermediate of pesticides, veterinary drugs, organic dyes and photosensitive materials, etc. It can be used to manufacture fungicide carbendazim, veterinary insect repellant albendazole, anti-aging agent MB and other products. There are two main preparation methods of o-nitroaniline: [0003] One is to use o-chloronitrobenzene as a raw material, react with a certain concentration of ammonia water in an autoclave to prepare o-nitroaniline. This method has been widely concerned by people in the 1930s, and has been studied in depth. Due to the cheap and easy-to-obtain raw materials, and the simple production operation, this preparation method is still commonly used in production plants. Due to the use of ammonia in the reaction process, a large amount of ammonium chloride-conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/10
Inventor 董传明褚吉成
Owner 凯美泰克(天津)化工科技有限公司
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