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Preparation method of high-loading rare and noble metal loaded carbon-based material

A technology of carbon-based materials and rare and precious metals, applied in structural parts, electrical components, battery electrodes, etc., can solve the problems of slow oxygen reduction reaction rate, limited Pt resources, cumbersome preparation process, etc., to improve the utilization rate of functional reactions, pores The effect of rich structure and large specific surface area

Pending Publication Date: 2022-02-15
CHANGCHUN GOLD RES INST
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  • Abstract
  • Description
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Problems solved by technology

However, Pt resources are limited and expensive, and the slow oxygen reduction reaction rate of the low-loaded Pt-based catalyst cathode cannot meet the commercial requirements of proton exchange membrane fuel cells.
In addition, due to the corrosion of the carrier in the carbon-supported nano-Pt particle catalyst, the dissolution, migration, and agglomeration of the nano-Pt particles into larger particles, the active sites of the oxygen reduction reaction are covered, which reduces the electrocatalytic activity.
Unlike traditional Pt / C catalysts used in chemical industry (Pt loading is less than 5wt%), Pt / C catalysts used in hydrogen-oxygen proton exchange membrane fuel cells generally have a noble metal Pt loading of more than 20wt%, and the preparation process is also very cumbersome

Method used

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  • Preparation method of high-loading rare and noble metal loaded carbon-based material
  • Preparation method of high-loading rare and noble metal loaded carbon-based material
  • Preparation method of high-loading rare and noble metal loaded carbon-based material

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preparation example Construction

[0034] A method for preparing a high-capacity rare metal-loaded carbon-based material, comprising the following steps:

[0035] Step 1, preparation of carbon-based support

[0036] Mix and stir the cobalt salt, chelating agent and organic phase solvent and disperse evenly, put it into a pressure melting bomb and heat up to a temperature of 100-150°C, react for 180-300min, wash, centrifuge, dry and grind after completion, Calcination and activation in a flowing atmosphere, cooling to room temperature and grinding to obtain a carbon-based carrier Co / C material;

[0037] Step 2, preparation of high-loaded rare metal carbon-based materials

[0038] Disperse the platinum salt solution, stabilizer and the carbon-based carrier Co / C material prepared in step 1 in the organic phase solvent and stir evenly, adjust the pH value to 9.0-11.0, add a reducing agent after stabilization, and wash, Filtration, drying, grinding, and then in a flowing atmosphere, the reduction product is activa...

Embodiment 1

[0053] A method for preparing a high-capacity rare metal-loaded carbon-based material, comprising the following steps:

[0054] Step 1: Dissolve cobalt nitrate hexahydrate, 2-aminoterephthalic acid, and triethylenediamine in N,N-dimethylacetamide solvent in a mass ratio (1:1:3), dissolve and disperse them Uniform; react at 140°C for 180min, cool to room temperature naturally, wash with ethanol three times, and dry at 60°C for 600min. Put the collected powder into a porcelain boat by grinding and place it in a tube furnace, calcinate and activate it under a nitrogen atmosphere and raise the temperature to 300°C at a rate of 5°C / min and keep it for 60min. After cooling to room temperature, take out the product and fully The carrier Co / C material is obtained after grinding.

[0055] Step 2, using chloroplatinic acid as the precursor of noble metal Pt, in reducing agent (KBH 4 )-Basic system, adopt impregnation-liquid phase reduction method to prepare high-loaded precious metal ...

Embodiment 2

[0060] Such as figure 1 , figure 2 and Figure 5 As shown, the present embodiment is the same as Example 1, the difference is that in step 1, cobalt nitrate hexahydrate, 2-aminoterephthalic acid, and triethylenediamine are dissolved in N by mass ratio (1:1:3). In N-dimethylacetamide solvent, make it dissolve and disperse evenly; react at 100°C for 200min, activate and calcinate the Co-doped carbon derived from MOF described in step 1 in a tube furnace at 500°C, keep warm The time is 30 minutes. In step 2, the pH value is adjusted to 9.0, and the reaction is carried out at 100°C for 300 minutes. In step 2, the sample obtained by washing, filtering, drying, and grinding after the constant temperature reaction is placed in a tube furnace, and the temperature is raised to 800°C under a nitrogen atmosphere for calcination. Activation heat treatment, the reaction time is 300min. The temperature was raised to 800°C at a rate of 30°C / min.

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Abstract

The invention belongs to the technical field of new energy materials and application, and particularly relates to a high-loading rare and noble metal loaded carbon-based material and a preparation method thereof.A Co / C carrier is prepared through a solvothermal-high-temperature calcination method, and Pt nanoparticles are loaded through an impregnation adsorption-liquid phase reduction method; and segmented heat treatment is performed on the obtained powder to obtain a black product, namely the high-loading rare and noble metal loaded carbon-based material. The rare and noble metal-loaded carbon-based material is synthesized and prepared by regulating and controlling the nucleation rate of metal nanocrystals and adopting an in-situ growth method, so that the wrapping of a carbon-based carrier loaded with rare and noble metal particles and the agglomeration of the nano rare and noble metal particles are effectively inhibited, and the utilization rate of single atoms participating in functional reaction is effectively improved; and the problem that a large number of rare and noble metal nanoparticles are wrapped due to mixing of conventional salt and a carbon source is effectively solved, meanwhile, the completeness of a carbon carrier material is effectively kept, and the situation that too many rare and noble metal nanoparticles are introduced into the carrier material and agglomerated, and the atom utilization rate is affected is avoided.

Description

technical field [0001] The invention belongs to the technical field of new energy materials and applications, and specifically relates to a preparation method of a high-capacity rare metal-loaded carbon-based material. Background technique [0002] Proton exchange membrane fuel cell has become an ideal power source for very attractive mobile portable devices and new energy electric vehicles due to its low carbon emissions, high energy density and simple structure. There is an overpotential in the cathode oxygen reduction reaction of proton exchange membrane fuel cells, and it is difficult to make the reaction occur without a catalyst, so a certain amount of active rare metal catalyst is required. At present, the most effective catalyst for proton exchange membrane fuel cells is still platinum (Pt)-based catalysts, because the noble metal Pt exhibits better O 2 Adsorption and dissociation characteristics, and then show high oxygen reduction reaction activity; at the same tim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/92H01M4/90H01M4/88
CPCH01M4/926H01M4/90H01M4/88Y02E60/50
Inventor 吴国玉郑晔邢志军
Owner CHANGCHUN GOLD RES INST