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
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[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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