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Method for preparing palladium carbon catalyst of high activity

A palladium-carbon catalyst, activated carbon technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Can not achieve hydrogenation and other problems, to achieve the effect of high hydrogenation catalytic activity, uniform grain distribution, and improved catalytic activity

Inactive Publication Date: 2009-05-20
CHANGSHA RONGXING NOBLE METAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The following phenomenon occurs in the 5% palladium carbon catalysts currently sold and used on the market: the indicated activity is greater than 95%, but the actual requirements do not meet the required standards, such as the catalytic hydrogenation of o-chloronitrobenzene to prepare 2,2-dichlorohydroazobenzene The yield is only 90 to 93%; the catalyst contains more metal impurities, and the ash content is mostly about 3%, which affects the product yield; the palladium is unevenly distributed, and some palladium is distributed in the inner pores of the activated carbon, which is not easy to contact with the reactants, and cannot achieve the desired effect. Hydrogen effect; palladium grains are large (5-20nm), palladium grains have superimposed crystal phenomenon, which affects hydrogenation activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Activated carbon pretreatment: mix 1.5M hydrochloric acid solution with activated carbon, the solid-to-liquid ratio is 4:1, stir at 60°C for 2 hours, wash with pure water until neutral; then use 0.1% H 2 o 2 Mix with activated carbon at a solid-to-liquid ratio of 4:1, stir at 40°C for 2 hours, filter, and dry at 120°C; finally mix with activated carbon with 0.2% polyvinyl alcohol solution at a solid-to-liquid ratio of 4:1, at 30°C Stir for 1 h, filter, and dry at 80° C.; the preparation process of the palladium solution is: weigh 1.68 Kg of palladium chloride, add 2.4 times of 6M hydrochloric acid to dissolve, and obtain H 2 PdCl 4 Solution, add polyethylene glycol equivalent to 0.1 times the amount of palladium substance, and then add water to dilute to 20L.

[0024] 2. Activated carbon loading: Weigh 19Kg of pretreated activated carbon, add 130L of pure water to make a slurry, raise the temperature to 60°C, add the prepared palladium solution at a speed of 80ml / m...

Embodiment 2

[0030] 1. Activated carbon pretreatment: mix 2M hydrochloric acid solution with activated carbon, the solid-to-liquid ratio is 5:1, stir at 70°C for 3 hours, wash with pure water until neutral; then use 0.2% H 2 o 2 Mix with activated carbon at a solid-to-liquid ratio of 5:1, stir at 50°C for 3 hours, filter, and dry at 120°C; finally mix with 0.3% polyvinyl alcohol solution and activated carbon at a solid-to-liquid ratio of 5:1, at 40°C Stir for 2 hours, filter, and dry at 80°C; the preparation process of the palladium solution is as follows: Weigh 1.68Kg palladium chloride, add 2.4 times of 6M hydrochloric acid to dissolve, and obtain H 2 PdCl 4 Solution, add polyethylene glycol equivalent to 1 times the amount of palladium substance, and then add water to dilute to 20L.

[0031] 2. Activated carbon loading: Weigh 19Kg of pretreated activated carbon, add 130L of pure water to make a slurry, raise the temperature to 60°C, add the prepared palladium solution at a speed of 80...

Embodiment 3

[0036] 1. Activated carbon pretreatment: mix 2.5M hydrochloric acid solution with activated carbon, the solid-to-liquid ratio is 6:1, stir at 80°C for 5 hours, wash with pure water until neutral; then use 0.3% H 2 o 2 Mix with activated carbon at a solid-to-liquid ratio of 6:1, stir at 60°C for 5 hours, filter, and dry at 120°C; finally mix 0.4% polyvinyl alcohol solution with activated carbon at a solid-to-liquid ratio of 6:1, and dry at 50°C Stir for 3 hours, filter, and dry at 80°C; the preparation process of the palladium solution is as follows: Weigh 1.68Kg palladium chloride, add 2.4 times 6M hydrochloric acid to dissolve, and obtain H 2 PdCl 4 Solution, add polyethylene glycol equivalent to 2 times the amount of palladium substance, and then add water to dilute to 20L.

[0037] 2. Activated carbon loading: Weigh 19Kg of pretreated activated carbon, add 130L of pure water to make a slurry, raise the temperature to 60°C, add the prepared palladium solution at a speed of...

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Abstract

The invention provides a method for preparing a high active palladium-carbon catalyst. The method comprises the following steps: palladium chloride is dissolved by hydrochloric acid to be prepared into a solution with certain concentration, then the solution is added into pretreated activated carbon along with an auxiliary agent to ensure that palladium is evenly dispersed on the surface and the subsurface of carbon, and then the high active palladium-carbon catalyst is obtained through the reduction of a reducing agent.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a preparation method of a highly active palladium carbon catalyst. Background technique [0002] The following phenomenon occurs in the 5% palladium carbon catalysts currently sold and used on the market: the indicated activity is greater than 95%, but the actual requirements do not meet the required standards, such as the catalytic hydrogenation of o-chloronitrobenzene to prepare 2,2-dichlorohydroazobenzene The yield is only 90 to 93%; the catalyst contains more metal impurities, and the ash content is mostly about 3%, which affects the product yield; the palladium is unevenly distributed, and some palladium is distributed in the inner pores of the activated carbon, which is not easy to contact with the reactants, and cannot achieve the desired effect. Hydrogen effect; palladium crystal grains are relatively large (5-20nm), and palladium crystal grains have superimposed cryst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J21/18
Inventor 陈建张治明黄周明
Owner CHANGSHA RONGXING NOBLE METAL
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