O-phenylenediamine preparation process by means of hydrogenization with nano nickel serving as catalyst

The technology of o-phenylenediamine and catalyst is applied in the field of preparation of o-phenylenediamine, which can solve the problems of long production cycle, poor product quality, large amount of waste water, etc., and achieve the effects of reducing corrosion, reducing energy consumption and reducing pollution

Inactive Publication Date: 2012-08-15
JIANGSU KANGHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the industrial production method of o-phenylenediamine is mainly based on the reduction of sodium sulfide: o-nitroaniline is placed in iron powder or sodium sulfide in the kettle, under acidic conditions, reacted at 80-90 ° C for 8-9 hours, alkalized, and cooled to obtain the crude product , and then rectified to obtain fine products, the yield is about 80%, and the purity is relatively poor, generally about 90%
Its disadvantages are large amount of waste water, long production cycle, low yield and poor product quality

Method used

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  • O-phenylenediamine preparation process by means of hydrogenization with nano nickel serving as catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 150 g of o-nitroaniline and 300 g of methanol into the autoclave, add 4.5 g of nano-nickel catalyst at the same time, close the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, ventilate 3 times, and adjust the pressure of the autoclave to 1.0 MPa, stir and heat up to 35-45°C to react, so that the pressure does not change (about 1h), take a sample, and the result of gas chromatography analysis shows that the content of o-phenylenediamine is 99.20%, (HPLC coupling compound 0.45%)

[0018] Comparative test:

[0019] Add 150 g of o-nitroaniline and 300 g of methanol into the autoclave, and add 7.5 g of ordinary Ni catalyst at the same time, close the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, change the air for 3 times, and adjust the pressure of the autoclave to 2.0 MPa, stir and heat up to 60-70°C to react, so that the pressure does not change (about 2-3h), take a sample, and the result of gas chromatography analysis sh...

Embodiment 2

[0021] Add 500 g of o-nitroaniline and 1,000 g of methanol into the autoclave, and add 15 g of nano-nickel catalyst at the same time, close the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, ventilate 3 times, and adjust the pressure of the autoclave to 1.0 MPa , stir and heat up to 35-45°C to react, so that the pressure does not change (about 1h), take a sample, and the result of gas chromatography analysis shows that the content of o-phenylenediamine is 99.18% (HPLC coupling compound 0.43%), after the reaction solution is filtered, the solvent is recovered, and then Rectification obtained 370g of white o-phenylenediamine, GC detection 99.9%, yield 94.5%

[0022] Comparative test:

[0023] Add 500 g of o-nitroaniline and 1000 g of methanol into the autoclave, and add 25 g of ordinary Ni catalyst at the same time, close the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, change the air for 3 times, and adjust the pressure of the aut...

Embodiment 3

[0025] Add 1,000 g of o-nitroaniline and 2,000 g of methanol into the autoclave, and at the same time add 30 g of nano-nickel catalyst, close the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, ventilate 3 times, and adjust the pressure of the autoclave to 1.0 MPa , stir and heat up to 35-45°C to react, so that the pressure does not change (about 1h), take a sample, and the result of gas chromatography analysis is that the content of o-phenylenediamine is 99.28% (HPLC coupling compound 0.40%), after the reaction solution is filtered, the solvent is recovered, and then Rectification obtained 745g of white o-phenylenediamine, GC detection 99.9%, yield 95.2%

[0026] Comparative test:

[0027] Add 1000 g of o-nitroaniline and 2000 g of methanol into the autoclave, and add 50 g of ordinary Ni catalyst at the same time, close the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, change the air for 3 times, and adjust the pressure of the aut...

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Abstract

The invention discloses an o-phenylenediamine preparation process by means of hydrogenization with nano nickel serving as a catalyst. The o-phenylenediamine is prepared by means of reduction process with ortho-nitroaniline serving as a raw material and alcohol serving as solvent. The process is characterized in that nano nickel and hydrogen which serve as catalysts are added during reaction, the hydrogen pressure ranges from 0.5MPa to 1.5MPa, the reaction temperature is below 30-80 DEG C, and the o-phenylenediamine is obtained by rectification after reduction for 0.5-10h. By means of the nano nickel catalyst with the patent application number being 201110059900.X and made by Jiangsu Kangheng chemical industry Co.,Ltd, the problem of a great quantity of organic waste water generated in reduction of iron powder or sodium sulfide in the traditional art is solved. The hydrogenization process avoids concentrated acid and concentrated base which are used in the traditional art, so that equipment corrosion is greatly reduced, pollution is reduced, and approximate zero pollution is achieved. Further, product yield and quality are improved, equipment production efficiency is improved, and energy consumption is greatly reduced.

Description

technical field [0001] The invention relates to a process for preparing o-phenylenediamine, in particular to a process for preparing o-phenylenediamine through a reduction process. Background technique [0002] O-phenylenediamine is an important intermediate of dyes, pesticides, additives, photosensitive materials, etc. Itself is the dye fur yellow brown M. Used in the manufacture of polyamide, polyurethane, fungicides carbendazim and thiophanate, vat red GG, leveling agent, anti-aging agent MB, also used in the preparation of developers, surfactants, etc. [0003] At present, the industrial production method of o-phenylenediamine is mainly based on the reduction of sodium sulfide: o-nitroaniline is placed in iron powder or sodium sulfide in the kettle, under acidic conditions, reacted at 80-90°C for 8-9h, alkalized, and cooled to obtain the crude product , and then rectified to obtain fine products, the yield is about 80%, and the purity is relatively poor, generally abou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/36
Inventor 邱志刚雍成松
Owner JIANGSU KANGHENG CHEM
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