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Solid phase interface induced precipitation method for preparing nickel oxide, cobalt oxide powder

A solid-phase interface, nickel oxide technology, applied in nickel oxide/nickel hydroxide, cobalt oxide/cobalt hydroxide and other directions, can solve the problems of coarse product particle size, difficult to achieve distribution, large solution volume, etc., and achieve fine product particle size, Easy operation and simple process effect

Inactive Publication Date: 2005-11-23
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This full-solution feeding method can only obtain rod-shaped or needle-shaped powder particles. The disadvantage is that the particle size of the product is coarse and uneven, and the particle size of the oxide powder is generally several microns; the fluidity of rod-shaped or needle-shaped particles is not good. When mixed with other powders or matrix materials, it is difficult to achieve sufficient and uniform distribution, which is not conducive to the stability and consistency of the final product quality
And these preparation methods are owing to adopting the whole solution state feeding mode, cause solution volume to be too large, have increased the processing burden of precipitation mother liquor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 1.0mol / L NiCl 2 Add 1.0 g of PVP dispersant to 500 mL of the solution, stir and mix evenly, adjust the pH of the solution to 4.5 with hydrochloric acid, and heat to 45°C; weigh 80.0 g of oxalic acid solid that has been broken and passed through 100 mesh, and add NiCl in three equal amounts 2 In the solution, each feed interval is 3 minutes, and the pH of the mixed solution is about 1.5. After the feeding was completed, the aging was continued for 0.5 hour; the stirring speed was controlled at 300 rpm during the feeding and aging process. After aging, filter and wash the powder with hot water until no anions can be detected in the washing liquid. After drying, 74.5g of nickel oxalate powder was obtained. The test and analysis results showed that the powder had a crystal structure, the particle size of the powder was between 0.5 and 20 μm, the average particle size was about 5 μm, and the microscopic shape was spherical or quasi-spherical.

[0015] The above nickel...

Embodiment 2

[0017] Take 1.0mol / L NiCl 2 Solution 500mL, add 1.0 g of OP dispersant, stir and mix evenly, adjust the pH of the solution to 4.5 with hydrochloric acid, and heat to 50°C; weigh 76.0 g of oxalic acid solid that has been broken and passed through 100 mesh, and add NiCl at one time 2 solution, the pH of the mixed solution is about 1.5 at this time. After the feeding was completed, the aging was continued for 0.5 hour; the stirring speed was controlled at 300 rpm during the feeding and aging process. After aging, filter and wash the powder with hot water until no anions can be detected in the washing liquid. After drying, 78.0 g of nickel oxalate powder was obtained. The test and analysis results showed that the powder had a crystal structure, the powder particle size was between 0.5 and 20 μm, the average particle size was about 3.5 μm, and the microscopic shape was spherical or quasi-spherical.

[0018] The above-mentioned nickel oxalate powder was calcined in an air atmosphe...

Embodiment 3

[0020] Take 1.5mol / L Ni(NO 3 ) 2 Solution 500mL, add 2.0 grams of OP dispersant, stir and mix evenly, and adjust the pH of the solution to 4.5 with nitric acid, and heat to 55°C; weigh 112.0 grams of ammonium oxalate solid that has been broken and passed 100 meshes, and add Ni(NO 3 ) 2 solution, the pH of the mixed solution at this time is about 1.0. After the feeding was completed, the aging was continued for 0.5 hour; the stirring speed was controlled at 200 rpm during the feeding and aging process. After aging, filter and wash the powder with hot water until the washing liquid is neutral. After drying, 115.5 g of nickel oxalate powder was obtained. The test and analysis results showed that the powder had a crystal structure, the powder particle size was between 0.5 and 20 μm, the average particle size was about 2.5 μm, and the microscopic shape was spherical or quasi-spherical.

[0021] The above-mentioned nickel oxalate powder was calcined in an air atmosphere at a tem...

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Abstract

The invention discloses a solid phase interface induced precipitation method for preparing nickel oxide, cobalt oxide powder, which comprises preparing 0.01-2.0mol / L solution from the soluble metal salt of the oxides to be prepared, charging macromolecular dispersing agent by the ratio of cobalt or nickel content of 0.1-1%, weighing oxalic acid or oxalates solid powder by the ratio of 1-1.2 times of metal cobalt or nickel, grinding and sifting, charging in within one time or for several times, controlling the reaction temperature to be 25-90 deg. C, adjusting pH to be 1.0-5.0, agitating at the speed of 100-300 mps, reacting and ageing 0.5-3 hours, producing insoluble metallic oxalate powder, finally 4-12 hours at 350-1000 deg. C, thus metallic oxide powder is prepared.

Description

technical field [0001] The invention relates to a preparation method of metal oxide powder. Specifically, it is a method for preparing nickel oxide and cobalt oxide powders by inducing precipitation at the solid phase interface. Background technique [0002] At present, the method of preparing metal oxide powder by wet chemical precipitation using oxalic acid or its salts is usually to pre-dissolve the metal salt and oxalic acid or oxalate to prepare a solution, and then mix, contact, and react under certain process conditions. Generate solid powder particles of a certain size and shape. For example, CN1114639A uses cobalt nitrate, nickel nitrate solution and ammonium oxalate solution to filter, wash and roast cobalt oxide and nickel oxide powder obtained after precipitation reaction; JP2208227A uses cobalt chloride solution as raw material, and oxalic acid or ammonium oxalate solution, precipitation, Cobalt oxide powder prepared by roasting with oxygen after filtration, w...

Claims

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Application Information

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IPC IPC(8): C01G53/04
Inventor 黄凯郭学益刘荣义李平刘晓剑卿波韩剑慧
Owner CENT SOUTH UNIV
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