Preparation method of o-phenylenediamine

A technology of o-phenylenediamine and o-nitroaniline, which is applied in the field of preparation of o-phenylenediamine, can solve the problems of reduced safety and cleanliness, increased equipment investment and energy consumption, and increased product post-processing procedures, so as to achieve easy operation , Improve production capacity, save equipment investment and production energy consumption

Inactive Publication Date: 2013-04-03
JIANGSU YANGNONG CHEM GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing catalytic hydrogenation process, no matter whether nickel is used as a catalyst or palladium / carbon is used as a catalyst, water or alcohols need to be added as a solvent. However, the use of solvents increases post-processing procedures such as product separation and solvent recovery. As a result, equipment investment and energy consumption increase, especially when alcohols with low boiling point and volatile are used as solvents, the safety and cleanliness of production are greatly reduced

Method used

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  • Preparation method of o-phenylenediamine
  • Preparation method of o-phenylenediamine
  • Preparation method of o-phenylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Coconut shell carbon with a particle size of 75 μm was used as the activated carbon carrier, and its specific surface area was 1500 m 2 / g, the ash content is 1.5%, weigh 50g of the above activated carbon, add 1000ml of 10wt% hydrochloric acid to it, heat and boil at 80°C for 4h, filter and wash with deionized water until neutral, filter and dry at 110°C. Add 400ml of 20wt% nitric acid to the dried activated carbon, heat and cook at 60°C for 4 hours, filter and wash with deionized water until neutral, filter, dry at 110°C, add 200ml of deionized water to the filter cake Prepared as charcoal slurry.

[0030] Weigh 1.67g of palladium chloride and 1.33g of chloroplatinic acid hexahydrate and dissolve them in 50ml of 20wt% dilute hydrochloric acid respectively, and mix the above two solutions to obtain 100ml of uniform metal salt mixture. Add it to the carbon slurry and stir at 30°C for 2 hours. At the same time, add 10% sodium carbonate to adjust the pH to 9.5. Continue t...

Embodiment 2

[0032] Apricot shell carbon with a particle size of 75 μm was used as the activated carbon carrier, and its specific surface area was 1200 m 2 / g, the ash content is 2%, weigh 50g of the above activated carbon, add 1000ml of 10wt% hydrochloric acid to it, heat and boil at 80°C for 4h, filter and wash with deionized water until neutral, filter and dry at 110°C. Add 400ml of 20wt% nitric acid to the dried activated carbon, heat and cook at 60°C for 4 hours, filter and wash with deionized water until neutral, filter, dry at 110°C, add 200ml of deionized water to the filter cake Prepared as charcoal slurry.

[0033]Weigh 1.67g of palladium chloride and 1.33g of chloroplatinic acid hexahydrate and dissolve them in 50ml of 20wt% dilute hydrochloric acid respectively, and mix the above two solutions to obtain 100ml of uniform metal salt mixture. Add it to the carbon slurry and stir at 30°C for 2 hours. At the same time, add 10% sodium hydroxide to adjust the pH to 9.6. Continue to s...

Embodiment 3

[0035] Coconut shell carbon with a particle size of 75 μm was used as the activated carbon carrier, and its specific surface area was 1500 m 2 / g, the ash content is 1.5%, weigh 50g of the above activated carbon, add 1000ml of 10wt% hydrochloric acid to it, heat and boil at 80°C for 4h, filter and wash with deionized water until neutral, filter and dry at 110°C. Add 400ml of 20wt% nitric acid to the dried activated carbon, heat and cook at 60°C for 4h, filter, wash with deionized water until neutral, filter, dry at 110°C, add 200ml of deionized water to make carbon slurry.

[0036] Weigh 2.0g of palladium chloride and 0.8g of chloroplatinic acid hexahydrate and dissolve them in 50ml of 20wt% dilute hydrochloric acid respectively, and mix the above two solutions to obtain 100ml of uniform metal salt mixture. Add it to the carbon slurry and stir at 30°C for 2 hours. At the same time, add 10% sodium carbonate to adjust the pH to 9.5. Continue to keep warm for 4 hours and then pa...

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Abstract

The invention provides a preparation method of o-phenylenediamine. In a hydrogenation reaction, ortho-nitroaniline is taken as a raw material, and water or organic solvents are not required to be added; under the existence of palladium-platinum bi-metallic catalyst taking activated carbon as a carrier, through series connection of multistage reaction kettles and under the conditions of the reaction temperature of 50 to 150 DEG C and the reaction pressure of 0.5 to 5 MPa, the continuous hydrogenation reduction reaction is carried out; and a reaction liquid flows through a film filtering system, concentrated size containing the catalyst returns to a first-stage reaction kettle, and the filtered clear o-phenylenediamine liquid is dehydrogenized and rectified to obtain the o-phenylenediamine finished product. Compared with the conventional process for preparing o-phenylenediamine through hydrogenation, the method provided by the invention has the advantages that equipment and energy consumption required in subsequent solvent recovery are saved, product quality is good, the production cost is low, the production capacity is high, and the operation is simple and convenient.

Description

technical field [0001] The invention relates to a method for preparing o-phenylenediamine, in particular to a method for preparing o-phenylenediamine by hydrogenation reduction using o-nitroaniline as a raw material. Background technique [0002] O-phenylenediamine is a white crystalline solid, which can be obtained by reduction of o-nitroaniline. It is mainly used in the production of benzimidazole fungicides, such as carbendazim and thiophanate-methyl. Suction-type carbendazim can prevent and control bacterial diseases of various crops, forest trees, fruits and vegetables, and preserve and store fruits and vegetables. In addition, o-phenylenediamine can also be used to prepare developer and surfactant. [0003] At present, there are mainly three methods for the industrial production of o-phenylenediamine in China: iron powder reduction, alkali sulfide reduction, and catalytic hydrogenation reduction. Although the production process of the first two routes is simple, the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/36
Inventor 袁源徐林顾志强丁克鸿戚明甫汪洋万宝坡李明
Owner JIANGSU YANGNONG CHEM GROUP
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