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Method for preparing carbon loading Pd nanometer particle catalyst by using homogeneous precipitation-reduction in situ method

A nanoparticle, homogeneous precipitation technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of Pd nanoparticle agglomeration and poor catalyst particle dispersion question

Inactive Publication Date: 2011-06-01
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the "local overconcentration" phenomenon during the addition of the reducing agent is likely to cause the agglomeration of Pd nanoparticles, resulting in poor dispersion of catalyst particles.

Method used

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  • Method for preparing carbon loading Pd nanometer particle catalyst by using homogeneous precipitation-reduction in situ method
  • Method for preparing carbon loading Pd nanometer particle catalyst by using homogeneous precipitation-reduction in situ method
  • Method for preparing carbon loading Pd nanometer particle catalyst by using homogeneous precipitation-reduction in situ method

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example 1

[0029] A method for preparing a carbon-supported Pd nanoparticle catalyst by homogeneous precipitation-in-situ reduction method, comprising the following steps:

[0030] 1. Weigh 60 mg of Vulcan XC-72R activated carbon powder from Cabot Company, add 3.13 ml 0.045 mol / L PdCl 2 solution, then adjust the pH value of the solution to 5.6~7.4, stir at high speed (or ultrasonic vibration) for 0.5~48 hours to make the mixture uniform, and heat in a water bath at 30~100°C for 2 hours.

[0031] 2. At room temperature (25°C), slowly add excess reducing agent solution (NaBH 4 ), mechanically stirred for 1 hour to completely react the metal salt with the reducing agent.

[0032] 3. After washing with water several times, check with silver nitrate solution until there is no chloride ion in the eluate. in N 2 Dry at 50°C under the same conditions to prepare a Pd / C catalyst with a metal loading of 20%, in which the particle size of the catalyst is about 2.0-4.0 nm.

[0033]

example 2

[0035] A method for preparing a carbon-supported Pd nanoparticle catalyst by homogeneous precipitation-in-situ reduction method, comprising the following steps:

[0036] 1. Weigh 60 mg of self-made carbon nanotubes (CNTs) with a tube diameter of 10-20nm, add 3.13 ml of 0.045 mol / L PdCl 2 , and then adjust the pH value of the solution to 5~7, and stir at high speed (or ultrasonic oscillation) for 0.5~48 hours to make the mixture uniform.

[0037]2. At room temperature (25°C), slowly add excess reducing agent solution (NaBH 4 ), mechanically stirred for 1 hour to completely react the metal salt with the reducing agent, and heated in a water bath at 30-100°C for 2 hours.

[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 The Pd / CNTs catalyst with a metal loading of 20% was obtained by drying at 50°C under atmospheric conditions, and the particle size of the catalyst was about 1.5-4.0nm.

...

example 3

[0041] A method for preparing a carbon-supported Pd nanoparticle catalyst by homogeneous precipitation-in-situ reduction method, comprising the following steps:

[0042] 1. Weigh 60 mg of carbon molecular sieve, add 3.13 ml 0.045 mol / L PdCl 2 solution, then adjust the pH value of the solution to 5~7, stir at high speed (or ultrasonic vibration) for 0.5~48 hours to make the mixture uniform, and heat in a water bath at 30~100°C for 2 hours.

[0043] 2. At room temperature (25°C), slowly add excess reducing agent solution (NaBH 4 ), mechanically stirred for 1 hour to completely react the metal salt with the reducing agent.

[0044] 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 atmospheric conditions, the carbon molecular sieve-supported Pd nanoparticle catalyst with a metal loading of 20% was prepared, and the particle size of the catalyst was about 2.0-4.0 nm.

[0045] ...

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Abstract

The invention discloses a method for preparing a Pd nanometer particle catalyst by using a homogeneous precipitation-reduction in situ method, which comprises the following steps of: adding a soluble PdII salt solution into a certain quantity of carbon carrier suspending solution; regulating pH of a mixture solution to be between 5.6 and 7.4; heating the solution at 30-100 DEG C; heating and hydrolyzing the soluble PdII salt solution to obtain a component A, i.e. carbon loading PdO.H2O nanometer particles; adding over-dose reducing agents into the component A and fully stirring so that the carbon loading PdO.H2O nanometer particles are fully reacted with the reducing agents; carrying out the reduction in-situ to obtain a component B; washing the component B; and drying the component B under the protection of vacuum or inert gases to obtain the carbon loading Pd nanometer particle (Pd / c) catalyst. The catalyst obviously improves the electro-catalysis performance of formic acid and shows excellent electro-catalysis activity and stability. The preparation method of the invention is simple and economic, and is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a preparation method of a direct formic acid fuel cell catalyst, in particular to a method of utilizing the principle of homogeneous precipitation-in-situ reduction through Pd II →PdO·H 2 O→Pd 0 Reaction Pathways Method for preparing carbon-supported Pd nanoparticle catalysts. Background technique [0002] Due to the advantages of high energy conversion efficiency and low environmental pollution, fuel cells will become the best "clean energy" in the future. Therefore, fuel cells have always been the focus of new energy development strategies. In recent years, direct formic acid fuel cells have attracted increasing attention because they can be used as power sources for electric vehicles and portable mobile power sources. Formic acid is in a liquid state at room temperature, has a low freezing point and is non-toxic, non-flammable, suitable for low-temperature work, and relatively safe. Direct formic acid fuel cells have ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44H01M4/88
CPCY02E60/50
Inventor 陈煜梁燕周益明唐亚文陆天虹
Owner JIANGSU DAOBO CHEM
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