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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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  • Abstract
  • Description
  • Claims
  • Application Information

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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 glycerol, and Reaction time and reaction temperature, to prepare nano-scale ultrafine palladium powder with smaller particle size and better dispersibility; glycerol is used as both reducing agent and dispersant, which reduces the introduction of impurities, simplifies the process, and is economical Environmental friendly

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

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Embodiment 1

[0019] Embodiment 1: a kind of preparation method of superfine palladium powder, concrete steps are as follows:

[0020] (1) Dissolve the palladium precursor (10mg palladium chloride) in hydrochloric acid-deionized water at a temperature of 25°C under stirring conditions to obtain a palladium precursor solution; wherein the palladium precursor solution in the palladium precursor solution (palladium chloride) The concentration is 0.005mol / L; the concentration of hydrochloric acid-hydrochloric acid in deionized water is 0.055mol / L;

[0021] (2) The palladium precursor solution is added dropwise in the glycerol, and the constant temperature reaction 10min obtains the palladium black solution at a stirring rate of 80°C and 500rpm at a temperature of 80°C; wherein the volume ratio of the palladium precursor solution to the glycerin is 1: 4;

[0022] (3) Aging the palladium black solution for 10 minutes, centrifuging the solid and liquid, removing the supernatant, washing the solid...

Embodiment 2

[0024] Embodiment 2: a kind of preparation method of superfine palladium powder, concrete steps are as follows:

[0025] (1) Under stirring conditions at a temperature of 25° C., the palladium precursor (10 mg palladium nitrate) is dissolved in hydrochloric acid-deionized water to obtain a palladium precursor solution; wherein the concentration of the palladium precursor (palladium nitrate) in the palladium precursor solution is 0.010mol / L; hydrochloric acid-hydrochloric acid concentration in deionized water is 0.085mol / L;

[0026] (2) The palladium precursor solution is added dropwise in the glycerol, and the constant temperature reaction 15min obtains the palladium black solution at a stirring rate of 120°C and 500rpm at a temperature of 120°C; wherein the volume ratio of the palladium precursor solution to the glycerol is 1: 2;

[0027] (3) Aging the palladium black solution for 15 minutes, centrifuging the solid and liquid, removing the supernatant, washing the solid with...

Embodiment 3

[0029] Embodiment 3: a kind of preparation method of superfine palladium powder, concrete steps are as follows:

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

[0031] (2) The palladium precursor solution is added dropwise in the glycerol, and the constant temperature reaction 20min obtains the palladium black solution at a temperature of 160° C. and a stirring rate of 500 rpm; wherein the volume ratio of the palladium precursor solution to the glycerol is 1: 3;

[0032] (3) Aging the palladium black solution for 20 minutes, centrifuging the solid and liquid, removing the supernatant, washing the solid with deionized water a...

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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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