Preparation method of superfine palladium powder

A technology of ultra-fine palladium powder and palladium black, applied in metal processing equipment, nanotechnology, transportation and packaging, etc., to achieve the effects of high product yield, easy industrial production, and reduced introduction of impurities

Pending Publication Date: 2022-01-21
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

[0004] The present invention aims at the problem of preparing superfine palladium powder by the existing chemical reduction method, proposes a kind of preparation method of superfine palladium powder, utilizes glycerol to reduce the palladium in the palladium precursor solution, by controlling the consumption of glyce

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  • Preparation method of superfine palladium powder
  • Preparation method of superfine palladium powder
  • Preparation method of superfine palladium powder

Examples

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Example Embodiment

[0019] Example 1: A method of preparing ultrafine palladium powder, the specific steps are as follows:

[0020] (1) At the temperature of 25 ° C, stirring conditions, the palladium precursor (1 mg of palladium chloride) is dissolved in hydrochloric acid-deionized water to obtain a palladium precursor solution; in which palladium precursor (palladium chloride) in the palladium precursor solution is The concentration of 0.005 mol / L; hydrochloric acid concentration in hydrochloric acid-deionized water is 0.055 mol / L;

[0021] (2) Palladium pre-migration solution was added dropwise to the propanol, and the constant temperature reaction was 10 min at a temperature of 80 ° C and 500 rpm. The palladium-black solution was obtained; wherein the volume ratio of the palladium precursor solution to the propylene glycol was 1: 4;

[0022] (3) The palladium-black solution is aged for 10 min, the solid-liquid centrifugation is separated, remove the supernatant, washing the solid to the upper...

Example Embodiment

[0024] Example 2: A method of preparing ultrafine palladium powder, the specific steps are as follows:

[0025] (1) At the temperature of 25 ° C, stirring conditions, the palladium precursor (palladium) is dissolved in hydrochloric acid-deionized water to obtain a palladium front-deionized water; wherein the concentration of palladium precursor (palladium nitrate) in the palladium precursor solution is 0.010 mol / L; hydrochloric acid concentration in hydrochloric acid - deionized water is 0.085 mol / L;

[0026] (2) Palladium pre-proliferation solution was added dropwise to the glycerol, and the constant temperature reaction was 15 min at a temperature of 120 ° C, 500 rpm to obtain a palladium-black solution; wherein the volume ratio of the palladium precursor solution to the propylene glycol was 1: 2;

[0027] (3) The palladium-black solution is aged for 15 min, the solid-liquid centrifugation is separated, remove the supernatant, washing the solid to the upper tank with deioniz...

Example Embodiment

[0029] Example 3: A method of preparing ultrafine palladium powder, the specific steps are as follows:

[0030] (1) At the temperature of 25 ° C, stirring conditions, the palladium precursor (10 mg of acetylacetonate palipate) is dissolved in hydrochloric acid-deionized water to obtain a palladium precursor solution; wherein the palladium precursor (acetylacetonate) in the palladium precursor solution is obtained. The concentration of 0.012 mol / L; hydrochloric acid concentration in hydrochloric acid - deionized water is 0.175 mol / L;

[0031] (2) Palladium pre-proliferation solution was added dropwise to the propanol, and the constant temperature reaction was 20 min at a temperature of 160 ° C, 500 rpm. The palladium-black solution was obtained; wherein the volume ratio of the palladium precursor solution to the propylene glycol was 1: 3;

[0032] (3) The palladium-black solution is expanded from 20 min, the solid-liquid centrifugation is separated, remove the supernatant, wash...

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Abstract

The invention relates to a preparation method of superfine palladium powder, and belongs to the technical field of precious metal material preparation. The method comprises the steps of dissolving a palladium precursor in hydrochloric acid-deionized water to obtain a palladium precursor solution; dropwise adding the palladium precursor solution into glycerol, and carrying out constant-temperature reaction for 10-30 minutes at the temperature of 80-200 DEG C to obtain a palladium black solution; and aging the palladium black solution for 10-30 minutes, carrying out solid-liquid separation, washing solid with deionized water and absolute ethyl alcohol, and carrying out vacuum drying to obtain the superfine palladium powder. According to the method, glycerol is used as a reducing agent and a dispersing agent, and the superfine palladium powder with the particle size of about 40nm is prepared by controlling the dosage of glycerol, the reaction time and the reaction temperature. The superfine palladium powder is good in dispersity, simple in preparation process, free of pollution, free of material waste, easy to wash and capable of being used for industrial production.

Description

technical field [0001] The invention relates to a preparation method of ultrafine palladium powder, which belongs to the technical field of preparation of precious metal materials. Background technique [0002] As a precious metal material, ultrafine palladium powder has excellent physical and chemical properties. At present, it is widely used in catalysts, conductive pastes, hydrogen storage materials and other fields. Extensive studies have shown that the smaller the particle size of palladium powder, the better its adsorption performance and electrical properties, and the catalytic activity will also increase. Therefore, the preparation process of ultrafine palladium powder is very important. [0003] At present, the preparation methods of ultrafine palladium powder mainly include chemical reduction method, electrochemical method and template method. The traditional preparation method of high ultra-fine palladium powder is chemical reduction method. The preparation proc...

Claims

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Application Information

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IPC IPC(8): B22F9/24B22F1/054B82Y40/00
CPCB22F9/24B82Y40/00
Inventor 郭一飞胡劲段云彪张维均王开军
Owner KUNMING UNIV OF SCI & TECH
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