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Method for preparing high-alloying carbon-supported PdFe nanocatalyst by in-situ reduction method

A nano-catalyst, alloyed carbon technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. Uniformity, uneven atomic distribution and other problems, to achieve the effect of high degree of alloying

Active Publication Date: 2011-08-31
LIANYUNGANG CCA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the extremely uneven atomic distribution of the prepared palladium-based composite metal precursor itself, high-temperature heat treatment still cannot effectively improve the uniformity of the catalyst from the perspective of atomic distribution, thereby preparing a highly uniform single-phase alloy
At the same time, high temperature treatment inevitably leads to the increase of the particle size of the metal nanoparticles, and leads to phase separation of the multi-element alloy under high temperature conditions, which reduces the catalytic efficiency of the catalyst.

Method used

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  • Method for preparing high-alloying carbon-supported PdFe nanocatalyst by in-situ reduction method
  • Method for preparing high-alloying carbon-supported PdFe nanocatalyst by in-situ reduction method
  • Method for preparing high-alloying carbon-supported PdFe nanocatalyst by in-situ reduction method

Examples

Experimental program
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example 1

[0030] The method for preparing high-alloyed carbon-supported PdFe nano-catalysts by in-situ reduction method comprises the following steps:

[0031] 1. Weigh 60 mg of Vulcan XC-72R activated carbon powder from Cabot Company, add 3.0 ml of 0.05 mol / L K to adjust the pH value to 1.0 ~ 6.0 2 PdCl 4 Solution, mechanically stirred or ultrasonically oscillated, add 2.0 ml 0.05 mol / L K at a pH of 1.0 to 6.0 at 30 to 100°C 3 Fe(CN)6 Solution, mechanically stirred for 2 to 72 hours to make the mixture uniform.

[0032] 2. At room temperature (25°C), slowly add excess reducing agent solution (NaBH 4 ), and mechanically stirred for 1 hour to completely react the palladium ferricyanide precursor with the reducing agent.

[0033] 3. After washing with water several times, check with silver nitrate solution until there is no chloride ion in the eluate. in N 2 Drying at 50°C under the same conditions can produce Pd with a metal loading of 20% and a PdFe atomic ratio of 3:2. 3 Fe 2 / C...

example 2

[0035] The method for preparing high-alloyed carbon-supported PdFe nano-catalysts by in-situ reduction method comprises the following steps:

[0036] 1. Weigh 60 mg of carbon nanotubes (CNTs) with a diameter of 10-20 nm, and add 3.0 ml of 0.05 mol / L K to adjust the pH value to 1.0 ~ 6.0 2 PdCl 4 Solution, mechanically stirred or ultrasonically oscillated, add 2.0 ml 0.05 mol / L K at a pH of 1.0 to 6.0 at 30 to 100°C 3 Fe(CN) 6 Solution, mechanically stirred for 2 to 72 hours to make the mixture uniform.

[0037] 2. At room temperature (25°C), slowly add excess reducing agent solution (NaBH 4 ), and mechanically stirred for 1 hour to completely react the palladium ferricyanide precursor with the reducing agent.

[0038] 3. After washing with water several times, check with silver nitrate solution until there is no chloride ion in the eluate. in N 2 Drying at 50°C under the same conditions can produce Pd with a metal loading of 20% and a PdFe atomic ratio of 3:2. 3 Fe 2 ...

example 3

[0040] The method for preparing high-alloyed carbon-supported PdFe nano-catalysts by in-situ reduction method comprises the following steps:

[0041] 1. Weigh 60 mg of carbon molecular sieve, add 3.0 ml of 0.05 mol / L K to adjust the pH value to 1.0 ~ 6.0 2 PdCl 4 Solution, mechanical stirring or ultrasonic vibration, at 30 ~ 100 ℃, add 1.5 mL 0.05 mol / L K 4 Fe(CN) 6 Solution, mechanically stirred for 2 to 72 hours to make the mixture uniform.

[0042] 2. At room temperature (25°C), slowly add excess reducing agent solution (NaBH 4 ), and mechanically stirred for 1 hour to completely react the palladium ferrocyanide precursor with the reducing agent.

[0043] 3. After washing with water several times, check with silver nitrate solution until there is no chloride ion in the eluate. in N 2 Drying at 50°C under the same conditions can produce graphene-supported Pd with a metal loading of 20% and a PdFe atomic ratio of 2:1. 2 Fe 1 Nanoparticle catalysts, in which the cataly...

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Abstract

The invention relates to a method for preparing a high-alloying carbon-supported PdFe nanocatalyst by an in-situ reduction method. The method comprises the following steps of: adding a soluble Pd<II> salt to a carbon support suspension, adding an Fe(CN)6<3-> or Fe(CN)6<4-> solution at 30-100 DEG C, controlling the mol ratio of the Pd<II> salt to the Fe(CN)6<3-> to be 1.5:1 or the mol ratio of the Pd<II> salt to the Fe(CN)6<4-> to be 2:1; fully stirring the mixture solution to obtain a component A, namely carbon-supported iron palladium prussiate or ferrous iron palladium prussiate nanoparticles; adding a reducing agent to the component A, fully stirring, reducing the nanoparticles in situ to obtain a component B; and washing with water and drying the component B to obtain the high-alloying carbon-supported PdFe nanocatalyst. The catalyst provided by the invention has obviously improved electrocatalytic performance on oxygen reduction and presents excellent electrocatalytic activity and stability. The preparation method provided by the invention is simple, economical and suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a method for preparing a direct methanol fuel cell catalyst, in particular to a method for preparing a highly alloyed carbon-supported PdFe nanometer particle catalyst designed from the atomic level and using an in-situ reduction method. Background technique [0002] Energy is closely related to the survival and development of human beings. With the depletion of fossil energy such as coal, oil, and natural gas, human beings are facing an energy crisis, and the use of fossil energy also causes serious environmental pollution. The inevitable choice for sustainable development. Due to the advantages of high energy conversion efficiency and low environmental pollution, fuel cells will become the best "clean energy" in the future. [0003] Because the direct methanol fuel cell (DMFC) has the advantages of simple structure, high energy density, abundant fuel sources, good storage and transportation safety, low pollution, high energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89H01M4/92B82Y40/00
CPCY02E60/50
Inventor 唐亚文张帼杰陈煜周益明陆天虹
Owner LIANYUNGANG CCA CHEM CO LTD
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