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Preparation method of palladium-platinum bimetallic catalyst

A bimetallic catalyst, palladium-platinum technology, applied in the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, amino compound preparation, etc., can solve the problem of selectivity decline in conversion rate, increase product post-treatment process, Improve the activity and life, save equipment investment and production energy consumption, and facilitate industrial production

Inactive Publication Date: 2013-05-01
JIANGSU YANGNONG CHEM GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the palladium / carbon catalysts used above all need to add water or alcohols as solvents in the process of preparing o-phenylenediamine by hydrogenation, and the use of solvents will increase post-treatment processes such as product separation and solvent recovery.
In addition, after the above-mentioned catalyst is applied mechanically, both the conversion rate and the selectivity have declined, resulting in an increase in the production cost of o-phenylenediamine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 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 the filter cake Prepared as charcoal slurry.

[0028] 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 to keep w...

Embodiment 2

[0031] 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-mentioned 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 the filter cake Prepared as charcoal slurry.

[0032] 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 charcoal 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...

Embodiment 3

[0035] Coconut shell carbon with a particle size of 106 μm was used as the activated carbon carrier, and its specific surface area was 1200 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 3.34g 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 9.3. Continue to stir and keep warm for 4 hours....

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Abstract

The invention relates to a preparation method of a palladium-platinum bimetallic catalyst. The preparation method is characterized by using active carbon as a carrier, pretreating the active carbon respectively by hydrochloric acid and nitric acid before preparation, then simultaneously loading palladium and platinum on the pretreated active carbon, and adding an activating agent into the active carbon with palladium and platinum for reduction to finally obtain the palladium-platinum bimetallic catalyst. According to the invention, the preparation method is simple; and the obtained palladium-platinum bimetallic catalyst disclosed herein has the advantages of high activity, long life, etc, and is especially suitable for preparing o-phenylenediamine by solvent-free hydrogenation.

Description

technical field [0001] The invention relates to a preparation method of a palladium-platinum bimetallic catalyst, in particular to a preparation method of a palladium-platinum bimetallic catalyst used for hydrogenating o-nitroaniline to prepare o-phenylenediamine. Background technique [0002] O-phenylenediamine is an important chemical intermediate, which can be used to produce benzimidazole fungicides, such as carbendazim and thiophanate-methyl. The traditional production process of o-phenylenediamine is alkali sulfide reduction, which has mature technology and simple process, but its "three wastes" are seriously polluted and the wastewater is difficult to treat. With the country's increasing emphasis on environmental protection issues, the process of preparing o-phenylenediamine by catalytic hydrogenation has developed rapidly in recent years, that is, o-phenylenediamine is obtained by catalytic hydrogenation reduction of o-nitroaniline in the presence of a catalyst. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C211/51C07C209/36
Inventor 袁源徐林顾志强丁克鸿戚明甫汪洋万宝坡
Owner JIANGSU YANGNONG CHEM GROUP
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