Method for preparing nano-palladium electro-catalyst by ethanol reduction

An electrocatalyst, nano-palladium technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve the problems of operator physical injury, complicated steps, high cost, and achieve simple and easy operation. , Good application prospect, low cost effect

Inactive Publication Date: 2013-01-16
ANHUI UNIV OF SCI & TECH
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Problems solved by technology

[0005] At present, there are many methods for preparing nano-palladium electrocatalysts, such as polyol reduction method, hydrothermal synthesis method, microwave radiation thermal decomposition method, photochemical synthesis method and seed crystal method, etc. Most of these methods have the following problems: ( 1) Due to the introduction of many chemical reagents such as chemical reducing agents, dispersion stabilizers, and coating agents, even toxic organic phases or simple alcohols are used as solvents, the product purification process is cumbersome, and the consumption of large additives may also bring certain environmental pollution; (2) Adding chemical reducing reagents such as polyol, formaldehyde, sodium borohydride or ascorbic acid, it is difficult to control the reduction rate, thus making it more difficult to control the shape; (3) Controlling the nano-morphology (4) The preparation process uses microwaves or high-energy radiation sources such as ultraviolet light and gamma radiation, which not only cause harm to the operator's body, but also cost a lot. High, so there are certain limitations in application promotion
In this method, palladium chloride with poor solubility is prepared into chloropalladium acid with better solubility, thereby improving the solubility of palladium salt, but the palladium content is relatively reduced, and the experimental steps are complicated. In addition, reflux equipment is required, and the process conditions are relatively harsh. , not conducive to large-scale industrial production

Method used

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  • Method for preparing nano-palladium electro-catalyst by ethanol reduction
  • Method for preparing nano-palladium electro-catalyst by ethanol reduction
  • Method for preparing nano-palladium electro-catalyst by ethanol reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1、 Add 20 mL of water and 4 mL of ethanol to the reaction vessel, and stir to obtain a water-ethanol mixed solution system;

[0029] 2. Add PdCl in sequence 2 and SDS powder into the water-ethanol mixed solution system to configure a mixed system, which contains PdCl 2 and SDS concentrations were 7.04×10 -4 mol / L and 7.04×10 -4 mol / L, put the prepared solution on a constant temperature magnetic stirrer at 25°C and stir for 8 minutes, the color of the solution is light yellow;

[0030] 3. Place the evenly stirred reaction solution on a magnetic stirrer to stir and heat. Use N 2 Protection, control the reaction temperature at 70°C, react for 1.5 hours, obtain a black suspension, stop the reaction;

[0031] 4. The black precipitate obtained in the reaction solution was separated by centrifugation, washed with ethanol and acetone, and vacuum-dried at 40° C. for 24 hours to obtain the nano-palladium electrocatalyst.

[0032] 5. The transmission electron micrograph (TEM...

Embodiment 2

[0034] 1、 Add 20 mL of water and 4 mL of ethanol to the reaction vessel, and stir to obtain a water-ethanol mixed solution system;

[0035] 2. Add PdCl in sequence 2 and SDS powder into the water-ethanol mixed solution system to configure a mixed system, which contains PdCl 2 and SDS concentrations were 7.04×10-4 mol / L and 3.12×10 -2 mol / L, put the prepared solution on a constant temperature magnetic stirrer at 25°C and stir for 8 minutes, the color of the solution is light yellow;

[0036] 3. Place the evenly stirred reaction solution on a magnetic stirrer to stir and heat. Use N 2 Protection, control the reaction temperature at 70°C, react for 1.5 hours, obtain a black suspension, stop the reaction;

[0037] 4. The black precipitate obtained in the reaction solution was separated by centrifugation, washed with ethanol and acetone, and vacuum-dried at 40° C. for 24 hours to obtain the nano-palladium electrocatalyst.

[0038] 5. The average particle size of the nano-palla...

Embodiment 3

[0040] 1、 Add 20 mL of water and 4 mL of ethanol to the reaction vessel, and stir to obtain a water-ethanol mixed solution system;

[0041] 2. Add PdCl in sequence 2 and SDS powder into the water-ethanol mixed solution system to configure a mixed system, which contains PdCl 2 and SDS concentrations were 7.04×10 -4 mol / L and 7.04×10 -2 mol / L, put the prepared solution on a constant temperature magnetic stirrer at 25°C and stir for 8 minutes, the color of the solution is light yellow;

[0042] 3. Place the evenly stirred reaction solution on a magnetic stirrer to stir and heat. Use N 2 Protection, control the reaction temperature at 70°C, react for 1.5 hours, obtain a black suspension, stop the reaction;

[0043] 4. The black precipitate obtained in the reaction solution was separated by centrifugation, washed with ethanol and acetone, and vacuum-dried at 40° C. for 24 hours to obtain the nano-palladium electrocatalyst.

[0044] 5. The average particle size of the nano-pal...

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Abstract

The invention relates to a method for preparing a nano-palladium electro-catalyst by ethanol reduction. The method reduces PdCl2 (palladium chloride) to metal Pd (palladium) nano-particles by the aid of ethanol reduction and action of cosolvent, and includes the steps: firstly, preparing ethanol water; secondly, adding PdCl2 powder and protective agents into the ethanol water, feeding shielding gas, heating and stirring to enable palladium positive ions to generate reduction reaction so that the Pd nano-particles are obtained; and thirdly, performing centrifugal separation after reaction is finished to obtain black precipitates, and washing by ethanol and acetone prior to drying so that the nano-palladium electro-catalyst is obtained. The nano-palladium electro-catalyst is synthesized in one step in a normal-temperature environment by using the ethanol water as a solvent and utilizing the reduction action and the solvent effect of the ethanol without additionally adding chemical reduction agents such as ascorbic acid and by means of magnetic stirring and water-bath heating to guarantee solubility of the PdCl2. The method is low in cost, environment-friendly and simple and feasible in operation process, and the prepared nano-palladium electro-catalyst is high in yield and centralized in particle size distribution and has good application prospect.

Description

technical field [0001] The invention relates to a method for preparing nanoparticles, in particular to a method for preparing nano-palladium electrocatalyst by using ethanol reduction. [0002] Background technique [0003] Direct ethanol fuel cells (DEFCs) have attracted widespread attention due to the advantages of non-toxic, low-cost, and wide-ranging sources. Platinum (Pt) is recognized as the best catalyst for the electrochemical oxidation of alcohol, but the intermediate product of the electrochemical oxidation of ethanol is easily adsorbed on the Pt electrode, which poisons the catalyst and the catalytic performance quickly declines. In addition, Pt is expensive and resource-poor. Therefore, the design of direct alcohol fuel cells using non-Pt catalysts has attracted much attention, among which palladium (Pd) is considered as one of the important alternative materials. [0004] The main factors affecting the activity of nano-Pd catalysts in fuel cells are the parti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/03B22F9/24
Inventor 王艳丽谭德新张明旭彭勇军刘永峰晏莹张雪萍
Owner ANHUI UNIV OF SCI & TECH
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