Material layering process for reduced o-phenylenediamine

A technology of o-phenylenediamine and o-nitroaniline, which is applied to the purification/separation of amino compounds, the preparation of amino compounds, and the preparation of organic compounds, etc., which can solve the problems of large residue, labor time and labor, and poor operating environment , to achieve the effect of reducing distillation residue, increasing production capacity and reducing unit consumption

Active Publication Date: 2015-11-04
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The original process needs to cool down the high-temperature material, centrifuge after crystallization, and then carry out rectification. This process consumes a lot of man-hours and labor, and the residue after rectification is relatively large, and the on-site operating environment is poor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] First mix o-nitroaniline chloride with ammonia water, carry out ammonification reaction, and obtain o-nitroaniline; then transfer o-nitroaniline to the reduction pot, add alkali sulfide, and after reduction, the reduction pot contains mother liquor, o-phthalate Hydrate of amine and salt; the first classification layer: After the reduction reaction is completed, the temperature of the material is lowered to 85-90°C, and after the analysis is qualified, the material is pressed into the layered tank of the first classification layer with nitrogen gas of about 0.3MPa; The material inlet of the layered tank of the first graded layer has a built-in gas-liquid separator, and a funnel-shaped separation device is built in the middle; the upper discharge pipe of the layered tank of the first graded layer is kept warm with 80-85°C hot water; the layered layer of the first graded layer The upper part of the tank is equipped with an external coil, and the lower part is equipped with ...

Embodiment 2

[0019] First mix o-nitroaniline chloride with ammonia water, carry out ammonification reaction, and obtain o-nitroaniline; then transfer o-nitroaniline to the reduction pot, add alkali sulfide, and after reduction, the reduction pot contains mother liquor, o-phthalate Hydrate of amine and salt; the first classification layer: After the reduction reaction is completed, the temperature of the material is lowered to 85-90°C, and after the analysis is qualified, the material is pressed into the layered tank of the first classification layer with nitrogen gas of about 0.3MPa; The material inlet of the layered tank of the first graded layer has a built-in gas-liquid separator, and a funnel-shaped separation device is built in the middle; the upper discharge pipe of the layered tank of the first graded layer is kept warm with 80-85°C hot water; the layered layer of the first graded layer The upper part of the tank is equipped with an external coil, and the lower part is equipped with ...

Embodiment 3

[0021] First mix o-nitroaniline chloride with ammonia water, carry out ammonification reaction, and obtain o-nitroaniline; then transfer o-nitroaniline to the reduction pot, add alkali sulfide, and after reduction, the reduction pot contains mother liquor, o-phthalate Hydrate of amine and salt; the first classification layer: After the reduction reaction is completed, the temperature of the material is lowered to 85°C, and after the analysis is qualified, the material is pressed into the layered tank of the first classification layer with 0.3MPa nitrogen; the first classification There is a built-in gas-liquid separator in the material inlet of the layered layer tank, and a built-in funnel-shaped separation device in the middle; the upper discharge pipe of the layered tank of the first layer is kept warm with 80°C hot water; the upper part of the layered tank of the first layer is equipped with an external disk tube, the lower part has a built-in coil (with cold and hot media);...

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PUM

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Abstract

The present invention provides a material layering process for reduced o-phenylenediamine. The process comprises: firstly, mixing o-nitrochlorobenzene and ammonia to acquire o-nitroaniline; then adding sodium sulphide to the o-nitroaniline, wherein after reduction, a reduction pot contains a hydrate of a mother solution, o-phenylenediamine and a salt; and separating the o-phenylenediamine by using a two-stage separation technique. The present invention employs the self-developed technique for layering reduced o-phenylenediamine, thereby reducing the energy consumption, shortening the man-hour, reducing the rectification residues, providing the necessary condition for subsequent smooth rectification, and acquiring the o-phenylenediamine with high quality; providing a basis for increasing productivity of carbendazim; further improving the product quality of the o-phenylenediamine and the recovery rate in production process, reducing unit consumption, and reducing costs;and improving the operating environment and greatly reducing the labor intensity.

Description

technical field [0001] The invention relates to the field of pesticide production, in particular to a material layering process after reduction of o-phenylenediamine. Background technique [0002] Because o-phenylenediamine is a traditional fine chemical intermediate, it is mainly used in the production of pesticides and is the raw material for the preparation of carbendazim and thiophanate-methyl. Its application in medicine has also been reported in the literature. The synthesis of o-phenylenediamine mainly uses o-nitrochlorinated benzene and ammonia to synthesize o-nitroaniline, and then reduces it to o-phenylenediamine with alkali sulfide. After the reduction, the material is layered, and the hydrate of o-phenylenediamine and salt in the upper layer is heated and desalted, and then sent to the carbendazim workshop for rectification. [0003] The original process needs to cool down the high-temperature material, centrifuge after crystallization, and then carry out recti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/36C07C209/86
Inventor 郑宏亮刘建清沈国宝喻宝琴姚周平高焰兵
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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