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Method for preparing carbon-supported palladium or palladium-platinum electro-catalyst for direct formic acid fuel cell under auxiliary protection of inorganic salt

A formic acid fuel cell and electrocatalyst technology, applied in the direction of catalyst activation/preparation, battery electrodes, chemical instruments and methods, etc., can solve the problems of poor dispersion of electrocatalysts, complex processes, energy consumption, etc., to reduce production energy consumption, simplify Process, the effect of reducing the amount of use

Active Publication Date: 2014-04-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since borohydride is a strong reducing agent, the reduction is fast, and the prepared electrocatalyst has poor dispersion
[0005] Chinese invention patent ZL200710043391.5 discloses "a method for preparing nano-palladium or palladium-platinum alloy electrocatalysts for fuel cells". Treatment removal, complex and energy-intensive process

Method used

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  • Method for preparing carbon-supported palladium or palladium-platinum electro-catalyst for direct formic acid fuel cell under auxiliary protection of inorganic salt
  • Method for preparing carbon-supported palladium or palladium-platinum electro-catalyst for direct formic acid fuel cell under auxiliary protection of inorganic salt
  • Method for preparing carbon-supported palladium or palladium-platinum electro-catalyst for direct formic acid fuel cell under auxiliary protection of inorganic salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1 gram of 99% palladium dichloride (PdCl 2 ) was dissolved in 50 mL of water to prepare a 0.1117 mol / L (containing palladium 11.9 mg / mL) aqueous solution, and 3 mL of the above PdCl 2 Aqueous solution, add 97 mL of deionized water, add 143 mg of XC-72 carbon carrier, alternately sonicate and stir to form a suspension, and then add 249.8 mg of KCl (molar ratio: KCl / PdCl 2 =10:1) and 65mg citric acid (molar ratio: citric acid / PdCl 2 =1:1), adjust the pH value to 9; then reflux the above mixed solution in an oil bath at 90°C for 10 hours, filter with suction after cooling, wash the filter cake with deionized water, dry in vacuum, and grind to obtain carbon-loaded Palladium electrocatalyst for fuel cells, wherein the mass percentage of active component palladium is 20% (Pd / C). Electrochemical test results (see image 3 , Figure 4 ): The stripping voltammetry curve of carbon monoxide (CO) shows that the peak potential of CO oxidation is 0.69 V; the current densit...

Embodiment 2

[0027] 1 gram of 99% palladium dichloride (PdCl 2 ) was dissolved in 50 mL of water to prepare an aqueous solution of 0.1117 mol / L (containing palladium 11.9 mg / mL), and 1 g of chloroplatinic acid (H 2 PtCl 6 ·6H 2 O) Dissolve in 50mL of water to prepare a 0.0386mol / L (containing platinum 7.4 mg / mL) aqueous solution. Take 3mL of the above PdCl 2 aqueous solution and 8.7 mL H 2 PtCl 6 ·6H 2 O aqueous solution, add 88mL of deionized water, add 234mg of XC-72 carbon carrier, alternately sonicate and stir to form a suspension, and then add 717mg of NH to the suspension 4 Cl (molar ratio: NH 4 Cl / PdCl 2 +H 2 PtCl 6 =20:1) and 322mg citric acid (molar ratio: citric acid / PdCl 2 + H 2 PtCl 6 =2.5:1), adjust the pH value to 10; then reflux the above mixed solution in an oil bath at 95°C for 6 hours, filter with suction after cooling, wash the filter cake with deionized water, dry it in vacuum, and get the carbon-loaded Fuel cell palladium electrocatalyst, wherein the mas...

Embodiment 3

[0029] 1 gram of 99% palladium dichloride (PdCl 2 ) was dissolved in 50 mL of water to prepare an aqueous solution of 0.1117 mol / L (containing palladium 11.9 mg / mL), and 1 g of chloroplatinic acid (H 2 PtCl 6 ·6H 2 O) Dissolve in 50mL of water to prepare a 0.0386mol / L (containing platinum 7.4 mg / mL) aqueous solution. Take 3mL of the above PdCl 2 aqueous solution and 4.3 mL H 2 PtCl 6 ·6H 2O aqueous solution, add 93mL deionized water, add XC-72 carbon carrier 104mg, alternately sonicate, stir to form a suspension, and then add 897mg KBr (molar ratio: KBr / PdCl 2 +H 2 PtCl 6 =15:1) and 489mg potassium citrate (molar ratio: potassium citrate / PdCl 2 + H 2 PtCl 6 =3:1), adjust the pH value to 9.5; then reflux the above mixed solution in an oil bath at 90°C for 8 hours, filter with suction after cooling, wash the filter cake with deionized water, dry it in vacuum, and get the carbon-loaded Fuel cell palladium electrocatalyst, wherein the mass percent of active component ...

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Abstract

The invention relates to a method for preparing a carbon-supported palladium or palladium-platinum electro-catalyst for a direct formic acid fuel cell under the auxiliary protection of inorganic salt. The method comprises the following steps of alternately and ultrasonically stirring a palladium or palladium-platinum precursor solution and a carbon carrier to form suspension, adding the inorganic salt and a reducing agent into the suspension, and adjusting the pH value to be 9 to 10; and performing refluxing for 6 to 10 hours at 90 to 100 DEG C in an oil bath, performing cooling and suction filtration, washing a filter cake, and performing vacuum drying and grinding to obtain the carbon-supported palladium or palladium-platinum electro-catalyst for the fuel cell, wherein the finally prepared carbon-supported palladium or palladium-platinum electro-catalyst for the fuel cell comprises 10 to 40 mass percent of metal active ingredients. The catalyst prepared by the method has a component particle size of 2.5 to 3nm, post-treatment is not required, and the method is easy to operate.

Description

technical field [0001] The invention belongs to the field of proton exchange membrane fuel cell electrocatalysts, and in particular relates to a preparation method of carbon-supported palladium or palladium-platinum direct formic acid fuel cell electrocatalysts with auxiliary protection of inorganic salts. Background technique [0002] Direct formic acid fuel cell has the advantages of non-toxic fuel, non-flammable, convenient storage and transportation, electrochemical activity, energy density, and higher proton conductivity than direct methanol fuel cell, and has lower permeability to proton exchange membrane. It can produce a large output power density and other advantages, and is considered by industry experts to be a fuel cell that is very promising to replace methanol fuel cells. [0003] In fuel cells, electrocatalysts play the role of electrochemical reaction "factories" and are the core materials in batteries. The development of electrocatalysts is one of the keys t...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J37/16H01M4/92
CPCY02E60/50
Inventor 曾建皇李目武韩明家杜丽廖世军
Owner SOUTH CHINA UNIV OF TECH
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