Method for preparing coated-type palladium carbon catalyst

A palladium-carbon catalyst and a coating-type technology are applied in the field of preparation of a coating-type palladium-carbon catalyst to achieve the effects of reduced pollution, simple preparation process and low price

Inactive Publication Date: 2016-05-04
ZHEJIANG METALLURGICAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Palladium carbon is a very commonly used noble metal catalyst, which can be used for nitro hydrogenation, alkyne reduction, Suzuki/Heck reaction, hydrogenation of benzene ring, hydroxyl oxidation, etc., but so far, ther

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0020] A kind of preparation method of coating type palladium carbon catalyst, this preparation method comprises the steps:

[0021] a) preparing palladium salt solution;

[0022] b) adding a certain amount of stabilizing agent and reducing agent in the palladium salt solution, making the palladium salt generate nano palladium suspension at a certain temperature;

[0023] c) After adding a certain amount of stabilizing agent in the nano-palladium suspension, continue to add the embedding agent solution, adjust the pH through the lye to hydrolyze the embedding agent, thereby making coated nano-palladium particles;

[0024] d) Finally, adding the coated nano-palladium particles into the activated carbon slurry to obtain a coated palladium-carbon catalyst.

[0025] In described step a), the palladium salt in the palladium salt solution is PdCl 2 , Pd(NO 3 ) 2 and Pd(OAc) 2 A kind of in; The solvent of palladium salt solution is a kind of in hydrochloric acid aqueous solution...

Embodiment

[0035] Embodiment: the preparation method of a kind of coated palladium carbon catalyst of the present invention, this preparation method comprises:

[0036] First use the palladium salt solution, under the action of the stabilizer, add the reducing agent to make the metal palladium example form a suspension of nano-palladium at a certain temperature, then add the stabilizer and the embedding agent, and adjust the pH to make the embedding agent completely Hydrolyze to generate corresponding oxides, then add to the carbon slurry, adjust the pH, and stir at a certain temperature for a certain period of time to prepare a coated palladium-carbon catalyst.

[0037] The specific surface of the gac used in the present invention is 100m 2 / g~4000m 2 / g, palladium salt is PdCl 2 , Pd(NO 3 ) 2 , Pd(OAc) 2 One of them; beat the activated carbon at 10℃~50℃ for 0.2h~3h, the solvent is deionized water or ethylene glycol, and the mass ratio of the solvent to the activated carbon is 4~7:...

Embodiment 1

[0039] Embodiment one: get 10gPdCl 2 The powder was stirred at 50°C for 3 hours in 800mL sodium chloride aqueous solution (containing 6.6g sodium chloride), and then cooled to room temperature. Trisodium citrate (73 g, 5 equiv) was added, stirred at 30° C. for 1 h, then 100 mL of reducing agent ethanol (30 equiv) was added, and stirred at 60° C. for 5 h. Cool to normal temperature, add stabilizer cetyltrimethylammonium bromide (82g, 4equiv), stir at 30°C for 1h, then add 400mL ethanol solution of tetraethylorthosilicate, which contains tetraethylorthosilicate (58g, 5equiv), after continuing to stir for 1h, use 5% sodium carbonate solution to adjust the pH to about 8.5, heat up to 50°C and stir for 2h, add 1450g carbon slurry (containing 291g of activated carbon), use 5% sodium carbonate solution to maintain The previous pH remained unchanged, and after stirring at 50° C. for 4 h, it was filtered.

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Abstract

A method for preparing a coated-type palladium carbon catalyst comprises the following steps: a) preparing a solution of a palladium salt; b) adding a certain amount of a stabilizer and a reducer into the solution of the palladium salt to form a nano palladium suspension at a certain temperature from the palladium salt; c) after adding a certain amount of the stabilizer into the nano palladium suspension, continuing to add a solution of an embedding agent, adjusting the pH with an alkali liquid for hydrolysis of the embedding agent to produce a coated nano palladium particles; and d) Finally, adding the coated nano palladium particles into active carbon charcoal slurry to obtain the coated-type palladium carbon catalyst; technical effects are that after metal palladium is coated, on one hand, loss, coalescing or poisoning of the metal palladium in a subsequent reaction process can be effectively reduced, on the other hand the coated-type palladium carbon catalyst has certain hydrophobic or hydrophilic effect, the use range and cycle times of the coated-type palladium carbon catalyst can be improved, the plant cost can be reduced, environmental pollution can be reduced, and the coated-type palladium carbon catalyst is more in line with the concept of green chemistry. The preparation method is simple and easy, raw materials are cheap and easily obtained, and the method is more suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a coated palladium-carbon catalyst, which belongs to the technical field of catalyst preparation. Background technique [0002] In recent years, precious metals have gradually become a research hotspot due to their unique applications in catalysis, gas sensors, fuel cells and other fields. However, due to the high surface energy of nano-noble metals, they are easy to aggregate or change their morphology, which will lead to a decrease in the catalytic activity and selectivity of metal particles. In order to reduce the aggregation of metal nanoparticles, people have been looking for new methods, such as the use of surfactants, to protect the surface of metal particles. For example, Copelin discloses a kind of Pd / SiO in European patent EP0009802 2 Catalyst and the method for preparing hydrogen peroxide by anthraquinone method, palladium catalyst is relatively stable in this process, probably because pallad...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J37/02B01J33/00
CPCB01J35/0006B01J21/18B01J31/0212B01J31/0275B01J33/00B01J37/0219B01J37/0221B01J37/0225
Inventor 潘剑明鞠景喜陈华魏小娟施春苗魏青
Owner ZHEJIANG METALLURGICAL RES INST
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