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Method for preparing nanometer cobalt powder by liquid-liquid two-phase method

A nano-cobalt and solution technology, applied in metal processing equipment, transportation and packaging, can solve the problems of difficult to control the final form of cobalt powder, complicated process control, and high requirements for equipment vacuum, achieving low cost, simple process, good looking effect

Inactive Publication Date: 2018-05-25
SICHUAN UNIV
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Problems solved by technology

This method is simple to operate, but requires high vacuum degree of equipment
Solution precipitation-reduction method, literature【Preparation Technology and Latest Development of Nano Cobalt Powder[R]. China Functional Materials and Industry Forum Conference Records, 2011. Zaizhi YANG, Xiaoming FU, Preparation Technology and Latest Development of Nano Cobalt Powder[R]. Proceedings of 2011 China Functional Materials Technology and Industry Forum (CFMTIF 2011)] introduced Yang Zaizhi, Fu Xiaoming and others with CoSO 4 solution and NaOH solution as raw materials, by mixing the two to obtain Co(OH) 2 Precipitate, then wash the precipitate, dry it, and reduce it with hydrogen to obtain nano-cobalt powder. This preparation method is that the shape and particle size of the cobalt powder are determined by the precipitation of the precursor, and it is not easy to control the final shape of the cobalt powder, and because hydrogen is used as the reducing agent, The reaction temperature is high, the energy consumption is large, and the equipment requirements are high
Microemulsion method, introduced in the literature [J.P.Chen, K.M.Lee, C.M.Sorensen.Magnetic Properties of microemulsionsynthesized cobalt fine particles[J].J.Appl.Phys.,1994,75(10):5876-5878]J.P.Chen et al. Dissolve the surfactant (sodium butylene diethylhexyl sulfonate) in isooctane first, then add CoCl 2 and NaBH 4 Dissolve in this solution at a certain concentration to obtain two kinds of microemulsions, mix the two kinds of microemulsions, use acetone and water as flocculants to coagulate the colloids, filter and wash with water to remove excess surfactant, and then mix the colloids Sent to dry to obtain nano-cobalt powder, but this method uses two kinds of microemulsions, the cost is higher, and the process control is more complicated, so that large-scale production is limited, and there is no detailed information about product morphology and particle size. describe

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  • Method for preparing nanometer cobalt powder by liquid-liquid two-phase method
  • Method for preparing nanometer cobalt powder by liquid-liquid two-phase method
  • Method for preparing nanometer cobalt powder by liquid-liquid two-phase method

Examples

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Embodiment 1

[0037] Dissolve cobalt chloride and sodium lactate in deionized water at 60°C, add stearic acid monoglyceride and stir to dissolve to obtain a 0.08mol / L cobalt complex solution, in which cobalt chloride, sodium lactate and stearic acid monoglyceride The molar mass ratio of the esters is 1:0.8:0.02. Mix n-pentane and n-propanol to form an organic solution, wherein the volume ratio of n-pentane and n-propanol is 1:0.5. Dissolve the cobalt complex solution prepared above in the prepared organic solution, add oleic acid, and stir magnetically until a uniform and stable cobalt microemulsion is formed, wherein the molar ratio of oleic acid to cobalt complex solution is 10 :1, the volume ratio of cobalt complex solution to organic solution is 1:8. Dissolve sodium borohydride and sodium hydroxide solution in deionized water at a molar ratio of 1:1 to prepare a sodium borohydride solution with a concentration of 1 mol / L. Measure the cobalt microemulsion and deionized water prepared a...

Embodiment 2

[0039] Dissolve cobalt sulfate and sodium malate in deionized water at 65°C, and add zinc stearate to stir and dissolve to obtain a 0.10mol / L cobalt complex solution, in which cobalt sulfate, sodium malate and zinc stearate The molar mass ratio is 1:1:0.03. Mix n-hexane and n-butanol to form an organic solution, wherein the volume ratio of n-hexane and n-butanol is 1:0.7. Dissolve the cobalt complex solution prepared above in the prepared organic solution, add sodium lauryl sulfate, and stir magnetically until a uniform and stable cobalt microemulsion is formed, wherein sodium lauryl sulfate is complexed with cobalt The molar ratio of the cobalt complex solution to the organic solution is 12:1, and the volume ratio of the cobalt complex solution to the organic solution is 1:10. Potassium borohydride and sodium hydroxide solution were dissolved in deionized water at a molar ratio of 1:2 to prepare an aqueous solution with a potassium borohydride concentration of 1.1 mol / L. Me...

Embodiment 3

[0041] Dissolve cobalt acetate and sodium citrate in deionized water at 70°C, and add polyvinylpyrrolidone to stir and dissolve to obtain a 0.12mol / L cobalt complex solution, wherein the molar mass of cobalt acetate, sodium citrate and polyvinylpyrrolidone The ratio is 1:1.2:0.03. Mix n-heptane and n-pentanol to form an organic solution, wherein the volume ratio of n-heptane and n-pentanol is 1:0.9. Dissolve the above-prepared cobalt complex solution in the prepared organic solution, add polyglycerol fatty acid ester, and stir magnetically until a uniform and stable microemulsion is formed, wherein the molar ratio of polyglyceryl fatty acid ester and cobalt complex solution The ratio is 13:1, and the volume ratio of cobalt complex solution to organic solution is 1:12. Dissolve sodium borohydride and sodium hydroxide solution in deionized water at a molar ratio of 1:3 to prepare an aqueous sodium borohydride solution with a sodium borohydride concentration of 1.3 mol / L. Measu...

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Abstract

The invention belongs to the technical field of preparing nanometer metal powder in metal functional materials, and relates to a method for preparing nanometer cobalt powder, in particular to a method for preparing nanometer cobalt powder by using a liquid-liquid two-phase method in an inverse microemulsion system. The method utilizes the ion balance between the organic phase and the water phase, and controls the reduction reaction of cobalt ions in the water solution through the inverse microemulsion. First prepare cobalt salt, complexing agent and dispersant into aqueous solution, and prepare W / O emulsifier, co-surfactant and organic solvent into organic solution; then mix the above two solutions to prepare inverse microemulsion ; Add reducing agent and initiator to reverse microemulsion and deionized water respectively, and mix under water bath heating conditions to form liquid-liquid two-phase reduction reaction. After the reaction, separate the product with a strong magnet, and repeatedly use ethanol and deionized water. Ultrasonic cleaning, vacuum freeze-drying, and finally a spherical cobalt powder with a smooth surface and a minimum average particle size of about 20nm.

Description

technical field [0001] The invention belongs to the technical field of preparing nanometer metal powder in metal functional materials, and relates to a method for preparing nanometer cobalt powder, in particular to a method for preparing nanometer cobalt powder by using a liquid-liquid two-phase method in an inverse microemulsion system. Background technique [0002] Nano-cobalt powder is an emerging functional material, which has the advantages of high catalytic activity, high surface activity, good sintering performance, high saturation magnetization, high signal-to-noise ratio, good oxidation resistance and high coercive force, etc. It is widely used in hard It can be used in high-quality alloys, magnetic liquids, permanent magnet materials, batteries, diamond tool manufacturing and other industries, and has shown many excellent properties in the fields of ceramics, catalysis, magnetic materials, hydrogen storage alloy electrodes and special coatings. [0003] In recent y...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B22F1/00
CPCB22F9/24B22F1/065B22F1/054
Inventor 龙沁李卓甘芸嘉王泽学谢克难
Owner SICHUAN UNIV
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