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Preparation method of monodisperse spherical porous palladium nano catalyst

A palladium nano- and monodisperse technology is applied in the field of preparation of nano-catalysts, which can solve problems such as inability to completely remove and affect catalytic applications, and achieve the effects of saving preparation costs, good prospects for industrial application and good controllability.

Inactive Publication Date: 2012-07-04
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Macromolecules are attached to the porous structure and cannot be completely removed, and they are distributed on the surface of the catalyst, covering the active sites and affecting catalytic applications
Recently, three-dimensional palladium nanostructures have attracted much attention, however, there are only a few reports on the synthesis of dendritic palladium nanostructures without additives.
Dendritic three-dimensional palladium nanodendrites can be successfully obtained by sonoelectrochemical method; high specific surface area, monodisperse dendritic palladium-platinum nanoparticles can be obtained by seed growth method, but this method requires polyhedral nano-palladium seeds

Method used

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  • Preparation method of monodisperse spherical porous palladium nano catalyst
  • Preparation method of monodisperse spherical porous palladium nano catalyst
  • Preparation method of monodisperse spherical porous palladium nano catalyst

Examples

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Embodiment 1

[0035] Preparation of monodisperse spherical porous palladium nanocatalyst: While vigorously stirring, add K 2 PdCl 4 Ascorbic acid solution (10-15mM) was added dropwise to the solution (2-4mM, 5mL) in an amount of 1-2mL. The prepared mixed solution was magnetically stirred (12000r / min) in an ice-water bath for 5-10min. Subsequently, the reaction solution was put into a 3 L ultrasonic cleaner, and the water temperature was kept at 40 °C. The ultrasonic reaction was carried out for 6 or 7 minutes (longer time is also acceptable), and the color of the solution turned brownish black. Separation by centrifugation (12000r / min, 5min), repeated washing with deionized water, and finally drying under vacuum or airflow protection for 6-7 hours (longer time is also acceptable) to obtain the product.

[0036] figure 1 For the SEM picture of the resulting product, it can be seen that the product is made of spherical particles without other by-products ( figure 1 a). Further enlarged ...

Embodiment 2

[0040] Change K 2 PdCl 4 The concentration of the solution was 1.25mM, and other conditions were the same as in Example 1.

Embodiment 3

[0042] Change K 2 PdCl 4 The concentration of the solution was 5.0 mM, and other conditions were the same as in Example 1.

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Abstract

A preparation method of a monodisperse spherical porous palladium nano catalyst comprises the following steps of: dripping an ascorbic acid solution, a formic acid solution or an acetic acid solution into a potassium tetrachloroplatinate solution with the concentration of 1.25-12.5mM which is put in an icy water bath while stirring, wherein the concentration of the ascorbic acid solution, the formic acid solution or the acetic acid solution is 10-15mM, the molar ratio of the potassium tetrachloroplatinate solution to the ascorbic acid solution, the formic acid solution or the acetic acid solution is 0.5: 1 to 3: 1; putting the reaction solution into an ultrasonic clearing machine and performing ultrasonic reaction, wherein the temperature of a water trough of the ultrasonic clearing machine is kept at 40 DEG C+ / -5 DEG C, the ultrasonic reaction lasts 10+ / -5 minutes, and the color the solution becomes brownish black; performing centrifugal separation; eluting with deionized water for multiple times; and drying in vacuum or in the protection of airflow to obtain the monodisperse spherical porous palladium nano catalyst. The catalytic activity of the obtained spherical porous palladium nanoparticle is twice of that of the commercial palladium black catalyst, with excellent catalytic stability; the perpetration method and the preparation device are simple, and easy to operate; andlarge-scale preparation can be easily realized.

Description

technical field [0001] The invention relates to a preparation method of a nano catalyst applied to a formic acid fuel cell, especially a preparation method of porous palladium nanospheres with good monodispersity (52nm average diameter), high specific surface area, high catalytic activity and long-term stability. Background technique [0002] The preparation of high-efficiency electrocatalysts is the key to ensure the improved performance and lifetime of electrochemical energy sources such as formic acid fuel cells. Transition metal nanostructures have attracted extensive attention in the development of electrocatalysts due to their unique catalytic and electrical properties. Platinum has been widely used as an electrocatalyst in formic acid fuel cells, however, the limited resources of platinum in nature and its low tolerance to carbon monoxide toxicity have prompted the search for its substitutes. The study found that palladium has excellent electrochemical catalytic acti...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J35/10H01M4/92
CPCY02E60/50
Inventor 唐少春孟祥康萨查冯歌王勇光任华
Owner NANJING UNIV
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