CN102059345A - Method for preparing cobalt-nickel metal or alloy powder by solution nebulization method - Google Patents
Method for preparing cobalt-nickel metal or alloy powder by solution nebulization method Download PDFInfo
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- CN102059345A CN102059345A CN 201010577129 CN201010577129A CN102059345A CN 102059345 A CN102059345 A CN 102059345A CN 201010577129 CN201010577129 CN 201010577129 CN 201010577129 A CN201010577129 A CN 201010577129A CN 102059345 A CN102059345 A CN 102059345A
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Abstract
The invention discloses a method for preparing cobalt-nickel metal or alloy powder by a solution nebulization method, which comprises the following steps of: preparing 0.1 to 3.0 mol/L solution from soluble cobalt salts or nickel salts or the mixture of the cobalt salts and the nickel salts, and adding the solution into an organic solvent soluble mutually with water for uniform mixing; introducing the solution into an airflow nebulizer in a special solution nebulization device, nebulizing the solution under the nebulization pressure of 1.0-2.5*105Pa by using an inert gas, introducing the nebulized solution into a vertical tubular electric furnace through a turbulence device, and performing reaction at the temperature of 750 to 950 DEG C to obtain the cobalt-nickel metal or alloy powder; and performing separation and recovery by using a two-stage high-efficiency retoclone collector and a one-stage cloth screen, and causing a sour gas in a gaseous phase to enter a leaching absorption tower for recycling. In the method, the cobalt-nickel metal or alloy powder with a complete crystal structure and a regular particle shape can be prepared by one step. Compared with the conventional process, the method greatly reduces the preparation cost, ensures a simple process flow, high powder preparation efficiency, high quality of product, an environmentally-friendly process and continuous automatic production, and is simple and convenient to operate.
Description
Technical field
The present invention relates to field of powder metallurgy.A kind of specifically solution atomization legal system is equipped with the method for nickel cobalt metal or alloy powder.
Background technology
The preparation method of nickel cobalt metal and alloy powder mainly contains metal bath atomization, carbonyl process, electrolysis, thermal decomposition method, reducing process etc. at present.Metal bath atomization production efficiency height is bar-shaped defective but the powder of preparation exists coarse size, pattern, has limited its application; The powder of electrolysis preparation is generally dendroid or needle-like, be not suitable for preparing spherical powder, and powder density is lower; The CO gas toxicity of using in the carbonyl process is very strong, so it requires very high to equipment; Thermal decomposition method is a raw material with high-purity oxalic acid cobalt and nickel oxalate generally, with CO
2Or N
2Do protection gas and decompose in heating furnace, this technology significantly reduces with respect to the hydrogen reduction method cost, and is relatively stricter but production control requires, and can not carry out large-scale production; Adopt the oxalates of hydrogen reducing nickel cobalt or the traditional handicraft route that oxide is the more employing of domestic enterprise, this method technology cost height, real income powder size are difficult to accurate control, and the microscopic appearance of powder is irregularly shaped and skewness more.Simultaneously these preparation methods all ubiquity technological process long, the production process complexity, the product size distribution is wayward, production efficiency low with shortcoming such as cost height.
Summary of the invention
The objective of the invention is to overcome above shortcoming, provide a kind of solution atomization legal system to be equipped with the method for nickel cobalt metal or alloy powder.Realizing the technological process square, but production process continuous automatic production simple to operate, the product size distribution is easy to control, and production efficiency is high and reduce cost.
The present invention includes following steps:
(1) mixture of soluble metal cobalt salt or nickel salt or nickel cobalt salt is mixed with the aqueous solution of 0.1～3.0mol/L, this aqueous solution is joined in the organic solvent that can dissolve each other with water mixes, the described aqueous solution and volume of organic solvent are than being 1:0.5～3;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using inert gas is 1.0～2.5 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in the solution atomization isolated plant enters into vertical tubular electric furnace again, is 750～950 ℃ in temperature, and reaction obtains nickel cobalt metal or alloy powder; Described solution atomization isolated plant is the applicant's a granted patent, referring to CN201361542Y;
(3) nickel cobalt metal or alloy powder separates recovery through two-stage efficient cyclone dust-precipitator with the one-level bagroom, and the acid gas in the gas phase enters the drip washing absorption tower and recycles.Described two-stage efficient cyclone dust-precipitator and one-level bagroom are prior art.
Described soluble metal cobalt salt or nickel salt are sulfate, chloride, nitrate.
The described organic solvent that can dissolve each other with water is alcohols, ketone, aldehydes.
Described inert gas is nitrogen, argon gas.
Advantage of the present invention: (l) one step of reaction finishes, and preparation technology is simply advanced, and preparation process is continuous, controlled, the metal recovery rate height, and supplementary product onsumption is few, and manufacturing cost reduces significantly than traditional handicraft, the production efficiency height; (2) He Cheng powder is even monodisperse particles, and the powder particle of preparation is evenly tiny, controllable size, and narrow diameter distribution, external morphology are evenly regular, can be used as the initial feed of new function material, are fit to the requirement of following advanced function Development of Materials; (3) Zhi Bei product quality height: because this method is easily accurately controlled the product chemical composition, can realize the mixing of atom level by the liquid phase mode, good reaction selectivity and can not introduce other impurity, the nickel cobalt (alloy) powder constituent element of preparation is evenly distributed, segregation-free, and the quality raw materials basis is established in the exploitation that can be new material; (4) sour gas in the product is recyclable, and no waste produces, environmentally safe; The process environmental protection, industrialization prospect is good.
Description of drawings
Fig. 1 is the microscopic appearance figure of embodiment 1 gained cobalt powder;
Fig. 2 is the XRD figure of embodiment 1 gained cobalt powder;
Fig. 3 is the microscopic appearance figure of embodiment 4 gained nickel powders;
Fig. 4 is the XRD figure of embodiment 4 gained nickel powders;
Fig. 5 is the microscopic appearance figure of embodiment 6 gained cobalt nickel powders;
Fig. 6 is the XRD figure of embodiment 6 gained cobalt nickel powders.
The specific embodiment
Embodiment 1:
(1) CoCl of configuration 1.0mol/L
2Solution, in the aqueous solution: the volume ratio of ethanol is that the ratio of 1:1 adds ethanol, mixes;
(2) solution is input in the pneumatic atomizer in the solution atomization isolated plant (authorized, the patent No. is CN201361542Y), using high pure nitrogen is 1.0 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in isolated plant enters into vertical tubular electric furnace again, and reaction obtains metal cobalt powder under temperature is 800 ℃;
(3) metal cobalt powder two-stage efficient cyclone dust-precipitator in prior art separates recovery with the one-level bagroom, and the drip washing absorption tower in prior art of the acid gas in the gas phase absorbs and obtains industrial dilute hydrochloric acid.
The gained powder detects through XRD, and product is single face-centered cubic crystal formation cobalt powder; By sem analysis, product is equally distributed sphere, and average grain diameter is 3.18 μ m; By chemical analysis, the metal cobalt powder oxygen content is 0.15%.
Embodiment 2:
(1) Co (NO of configuration 2.0mol/L
3)
2Solution, in the aqueous solution: the volume ratio of acetone is that the ratio of 1:3 adds acetone, mixes;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using high pure nitrogen is 1.5 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in isolated plant enters into vertical tubular electric furnace again, and reaction obtains metal cobalt powder under temperature is 850 ℃;
(3) metal cobalt powder separates recovery through two-stage efficient cyclone dust-precipitator in prior art with the one-level bagroom, and the drip washing absorption tower in prior art of the acid gas in the gas phase absorbs and obtains industrial dilute nitric acid.
The gained powder detects through XRD, and product is single face-centered cubic crystal formation cobalt powder; By sem analysis, product is equally distributed sphere, and average grain diameter is 2.75 μ m; By chemical analysis, the metal cobalt powder oxygen content is 0.10%.
Embodiment 3:
(1) CoSO of configuration 0.5mol/L
4Solution, in the aqueous solution: the volume ratio of methyl alcohol is that the ratio of 1:0.5 adds methyl alcohol, mixes;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using high pure nitrogen is 2.5 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in isolated plant enters into vertical tubular electric furnace again, and reaction obtains metal cobalt powder under temperature is 850 ℃;
(3) metal cobalt powder separates recovery through two-stage efficient cyclone dust-precipitator in prior art with the one-level bagroom, and the drip washing absorption tower in prior art of the acid gas in the gas phase absorbs and obtains industrial dilute sulfuric acid.
The gained powder detects through XRD, and product is single face-centered cubic crystal formation cobalt powder; By sem analysis, product is equally distributed sphere, and average grain diameter is 2.85 μ m; By chemical analysis, the metal cobalt powder oxygen content is 0.12%.
Embodiment 4:
(1) NiCl of configuration 2.0mol/L
2Solution, in the aqueous solution: the volume ratio of ethanol is that the ratio of 1:2 adds ethanol, mixes;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using high pure nitrogen is 1.5 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in isolated plant enters into vertical tubular electric furnace again, and reaction obtains metal nickel powder under temperature is 950 ℃;
(3) metal nickel powder two-stage efficient cyclone dust-precipitator in prior art separates recovery with the one-level bagroom, and the drip washing absorption tower in prior art of the acid gas in the gas phase absorbs and obtains industrial dilute hydrochloric acid.
The gained powder detects through XRD, and product is single face-centered cubic crystal formation nickel powder; By sem analysis, product is equally distributed sphere, and average grain diameter is 3.25 μ m; By chemical analysis, the metal nickel powder oxygen content is 0.17%.
Embodiment 5:
(1) NiSO of configuration 1.0mol/L
4Solution, in the aqueous solution: the ratio of the volume ratio 1:1 of formaldehyde adds formaldehyde, mixes;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using high-purity argon gas is 2.0 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in isolated plant enters into vertical tubular electric furnace again, and reaction obtains metal nickel powder under temperature is 950 ℃;
(3) metal nickel powder two-stage efficient cyclone dust-precipitator in prior art separates recovery with the one-level bagroom, and the drip washing absorption tower in prior art of the acid gas in the gas phase absorbs and obtains industrial dilute sulfuric acid.
The gained powder detects through XRD, and product is single face-centered cubic crystal formation nickel powder; By sem analysis, product is equally distributed sphere, and average grain diameter is 3.10 μ m; By chemical analysis, the metal nickel powder oxygen content is 0.12%.
Embodiment 6:
(1) CoCl of configuration 0.15mol/L
2The NiCl of solution and 0.35mol/L
2Solution mixes; Again in the aqueous solution: the ratio of the volume ratio 1:2.5 of ethanol adds ethanol, mixes;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using high pure nitrogen is 1.0 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in isolated plant enters into vertical tubular electric furnace again, and reaction obtains alloy powder under temperature is 850 ℃;
(3) alloy powder two-stage efficient cyclone dust-precipitator in prior art separates recovery with the one-level bagroom, and the drip washing absorption tower in prior art of the acid gas in the gas phase absorbs and obtains industrial dilute hydrochloric acid.
The gained powder detects through XRD, and product is the Ni of complete in crystal formation
7Co
3Alloy powder; By sem analysis, product is equally distributed sphere, and average grain diameter is 3.75 μ m; By chemical analysis, the alloy powder oxygen content is 0.10%.
Embodiment 7:
(1) CoCl of configuration 0.15mol/L
2The NiCl of solution and 0.35mol/L
2Solution mixes; Again in the aqueous solution: the ratio of the volume ratio 1:1 of formaldehyde adds formaldehyde, mixes;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using high pure nitrogen is 2.5 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in isolated plant enters into vertical tubular electric furnace again, and reaction obtains alloy powder under temperature is 900 ℃;
(3) alloy powder two-stage efficient cyclone dust-precipitator in prior art separates recovery with the one-level bagroom, and the drip washing absorption tower in prior art of the acid gas in the gas phase absorbs and obtains industrial dilute hydrochloric acid.
The gained powder detects through XRD, and product is the Ni of complete in crystal formation
7Co
3Alloy powder; By sem analysis, product is equally distributed sphere, and average grain diameter is 4.15 μ m; By chemical analysis, the alloy powder oxygen content is 0.15%.
Claims (3)
1. a solution atomization legal system is equipped with the method for nickel cobalt metal or alloy powder, it is characterized in that, may further comprise the steps:
(1) mixture of soluble metal cobalt salt or nickel salt or nickel cobalt salt is mixed with the aqueous solution of 0.1～3.0mol/L, this aqueous solution is joined in the organic solvent that can dissolve each other with water mixes, the described aqueous solution and volume of organic solvent are than being 1:0.5～3;
(2) solution is input to pneumatic atomizer in the solution atomization isolated plant, using inert gas is 1.0～2.5 * 10 at atomizing pressure
5Atomize under the Pa condition, the disturbing flow device in the solution atomization isolated plant enters into vertical tubular electric furnace again, is 750～950 ℃ in temperature, and reaction obtains nickel cobalt metal or alloy powder;
(3) nickel cobalt metal or alloy powder separates recovery through two-stage efficient cyclone dust-precipitator with the one-level bagroom, and the acid gas in the gas phase enters the drip washing absorption tower and recycles.
2. solution atomization legal system according to claim 1 is equipped with the method for nickel cobalt metal or alloy powder, it is characterized in that, described soluble metal cobalt salt or nickel salt are sulfate, chloride, nitrate.
3. solution atomization legal system according to claim 1 is equipped with the method for nickel cobalt metal or alloy powder, it is characterized in that, the described organic solvent that can dissolve each other with water is alcohols, ketone, aldehydes.
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| CN2010105771290A CN102059345B (en) | 2010-12-08 | 2010-12-08 | Method for preparing cobalt-nickel metal or alloy powder by solution nebulization method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105458278A (en) * | 2015-12-08 | 2016-04-06 | 贵研铂业股份有限公司 | Preparation method of high-purity spherical ruthenium powder |
| CN111842924A (en) * | 2020-07-16 | 2020-10-30 | 西安交通大学 | Microwave-assisted metal nanoparticle preparation method and system |
| CN115041696A (en) * | 2022-05-27 | 2022-09-13 | 禹州市新佳汇新材料科技有限公司 | Preparation method of NI-CO alloy material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002294312A (en) * | 2001-03-29 | 2002-10-09 | Toda Kogyo Corp | Method for manufacturing metal particle powder |
| CN101062524A (en) * | 2006-04-27 | 2007-10-31 | 昭荣化学工业株式会社 | Nickel powder manufacturing method |
| CN101497432A (en) * | 2009-03-12 | 2009-08-05 | 中南大学 | Method for preparing single or composite metal oxide by atomizing and oxidizing solution and special equipment |
| CN201361542Y (en) * | 2009-03-06 | 2009-12-16 | 中南大学 | Device special for atomizing and oxidizing solution |
-
2010
- 2010-12-08 CN CN2010105771290A patent/CN102059345B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002294312A (en) * | 2001-03-29 | 2002-10-09 | Toda Kogyo Corp | Method for manufacturing metal particle powder |
| CN101062524A (en) * | 2006-04-27 | 2007-10-31 | 昭荣化学工业株式会社 | Nickel powder manufacturing method |
| CN201361542Y (en) * | 2009-03-06 | 2009-12-16 | 中南大学 | Device special for atomizing and oxidizing solution |
| CN101497432A (en) * | 2009-03-12 | 2009-08-05 | 中南大学 | Method for preparing single or composite metal oxide by atomizing and oxidizing solution and special equipment |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105458278A (en) * | 2015-12-08 | 2016-04-06 | 贵研铂业股份有限公司 | Preparation method of high-purity spherical ruthenium powder |
| CN111842924A (en) * | 2020-07-16 | 2020-10-30 | 西安交通大学 | Microwave-assisted metal nanoparticle preparation method and system |
| CN115041696A (en) * | 2022-05-27 | 2022-09-13 | 禹州市新佳汇新材料科技有限公司 | Preparation method of NI-CO alloy material |
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