CN102601379A - Method for preparing porous spherical nickel powder - Google Patents
Method for preparing porous spherical nickel powder Download PDFInfo
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- CN102601379A CN102601379A CN2012100870072A CN201210087007A CN102601379A CN 102601379 A CN102601379 A CN 102601379A CN 2012100870072 A CN2012100870072 A CN 2012100870072A CN 201210087007 A CN201210087007 A CN 201210087007A CN 102601379 A CN102601379 A CN 102601379A
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- oxalate
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Abstract
A method for preparing porous spherical nickel powder relates to a method for preparing spherical nickel powder for powder metallurgy. The method is characterized in that soluble nickel salt solution reacts with ammonium oxalate solution to obtain spherical nickel oxalate, and then the obtained spherical nickel oxalate is in hydrogen disoxidation to obtain the porous spherical nickel powder. The spherical nickel powder prepared by the method has a porous surface and large specific surface area, and can meet the requirements of special industries.
Description
Technical field
A kind of preparation method of cellular globular powdered nickel relates to a kind of preparation method of powder used in metallurgy globular powdered nickel.
Background technology
Nickel powder is widely used in industries such as atomic energy industry, alkaline storage battery, electrical alloy, superalloy, catalyst and additive for powder metallurgy, secondary cell.The required nickel powder of existing market mainly contains electrolytic nickel powder and chemical nickel powder.The nickel powder microscopic appearance that electrolysis is produced is flourishing dendroid, and the nickel powder of chemical method preparation is because of producing the difference of process control, not only granularity can from tens microns to nanometer, and microscopic appearance also bigger difference can occur.Because the difference of microscopic appearance causes its character in application also to be very different, therefore pass through the pattern of control presoma, and obtain the nickel powder of different-shape.The cellular globular powdered nickel is not only spherical in shape, and the surface is cellular, has increased specific area greatly, can satisfy the demand of special industry.
At present, the method for preparing globular powdered nickel mainly contains aqueous phase precipitation reducing process, coordination precipitation direct-reduction process.The former generates nickel hydroxide with nickelous sulfate and NaOH reaction, makes globular powdered nickel with hydrazine hydrate reduction, and the shortcoming of this method is the large usage quantity of hydrazine hydrate, and cost is higher, and the sphericity of the globular powdered nickel that makes is uncontrollable.The latter is to be that precipitating reagent, nickel chloride are that raw material, ammonia are complexant with carbonic hydroammonium, is equipped with globular powdered nickel presoma deposition with the coordination precipitation legal system, and the presoma that in hydrogen reduction atmosphere, directly reduces again prepares the spherical super fine nickel powder.Adopt the sphericity of the globular powdered nickel that this method makes controlled, but presoma prepares and be prone in the process produce double salt, influence the quality of globular powdered nickel, adopt this method higher simultaneously, can only use nickel chloride or nickel nitrate the nickel ingredient requirement.
No matter adopt above-mentioned which kind of method, all can't prepare the cellular globular powdered nickel.
Summary of the invention
The object of the invention is exactly the deficiency that exists to above-mentioned prior art, provides a kind of not only spherical in shape, and the surface is cellular, can increase the preparation method of the cellular globular powdered nickel of specific area greatly.
The objective of the invention is to realize through following technical scheme.
A kind of preparation method of cellular globular powdered nickel; It is characterized in that its preparation process is that soluble nickel salting liquid and ammonium oxalate solution are reacted; Obtain spherical nickel oxalate, carry out hydrogen reducing to the spherical nickel oxalate that makes then, make the cellular globular powdered nickel.
The preparation method of a kind of cellular globular powdered nickel of the present invention is characterized in that described soluble nickel salt is a kind of in nickelous sulfate, nickel chloride or the nickel nitrate.
The preparation method of a kind of cellular globular powdered nickel of the present invention; It is characterized in that it is 50～70g/L that described soluble nickel salting liquid and ammonium oxalate solution carry out course of reaction nickel salt solution concentration, the volumetric concentration of ammonium oxalate solution is 40～60%, logical liquefied ammonia regulator solution pH to 7.5～8.5 during reaction; Under agitation add ammonium oxalate solution; Nickel content≤0.5g/L is terminal point in supernatant, and filtration washing obtains spherical nickel oxalate product after the drying.
The preparation method of a kind of cellular globular powdered nickel of the present invention is characterized in that under the situation of 300-450 ℃ of also logical hydrogen, carrying out reductase 12-3h to the spherical nickel oxalate that makes, and obtains the cellular globular powdered nickel after the cooling.
The preparation method of a kind of cellular globular powdered nickel of the present invention, the nickel powder of preparation is spherical in shape, and the surface is cellular, and bigger serface is big, can satisfy the demand of special industry.
The specific embodiment
A kind of preparation method of cellular globular powdered nickel, its process select any one nickel salt in nickelous sulfate, nickel chloride or the nickel nitrate for use, are mixed with the nickel solution of 50～70g/L, and ammonium oxalate also is mixed with 40～60% solution.Be heated to 40～60 ℃ to solution containing nickel, about logical liquefied ammonia regulator solution pH to 8, under agitation add ammonium oxalate solution fast, nickel content≤0.5g/L is terminal point in supernatant, and filtration washing obtains cellular globular powdered nickel product after the drying.Then the cellular globular powdered nickel that makes, under the situation of 300-450 ℃ and logical hydrogen, reduce about 2-3h, can obtain the cellular globular powdered nickel after the cooling.
Embodiment 1
With the nickelous sulfate is raw material, is mixed with the nickel solution of 58.32g/L, and ammonium oxalate also is mixed with 50% solution.Be heated to 50 ℃ to solution containing nickel, about logical liquefied ammonia regulator solution pH to 8, under agitation add ammonium oxalate solution fast, nickel content≤0.5g/L is terminal point in supernatant, and filtration washing obtains cellular globular powdered nickel product after the drying.The back is the cellular globular powdered nickel that makes, under the situation of 400 ℃ and logical hydrogen, reduces about 2.5h, and the specific area that obtains the cellular globular powdered nickel is 18.23m
2/ g.
Embodiment 2
With the nickelous sulfate is raw material, is mixed with the nickel solution of 50.49g/L, and ammonium oxalate also is mixed with 40% solution.Be heated to 40 ℃ to solution containing nickel, about logical liquefied ammonia regulator solution pH to 8, under agitation add ammonium oxalate solution fast, nickel content≤0.5g/L is terminal point in supernatant, and filtration washing obtains cellular globular powdered nickel product after the drying.Then the cellular globular powdered nickel that makes, under the situation of 300 ℃ and logical hydrogen, reduce about 2h, the specific area that obtains the cellular globular powdered nickel is 17.57 m
2/ g.
Embodiment 3
With the nickelous sulfate is raw material, is mixed with the nickel solution of 69.20g/L, and ammonium oxalate also is mixed with 60% solution.Be heated to 60 ℃ to solution containing nickel, about logical liquefied ammonia regulator solution pH to 8, under agitation add ammonium oxalate solution fast, nickel content≤0.5g/L is terminal point in supernatant, and filtration washing obtains cellular globular powdered nickel product after the drying.Then the cellular globular powdered nickel that makes, under the situation of 450 ℃ and logical hydrogen, reduce about 3h, the specific area that obtains the cellular globular powdered nickel is 18.72 m
2/ g.
Claims (4)
1. the preparation method of a cellular globular powdered nickel; It is characterized in that its preparation process is that soluble nickel salting liquid and ammonium oxalate solution are reacted; Obtain spherical nickel oxalate, carry out hydrogen reducing to the spherical nickel oxalate that makes then, make the cellular globular powdered nickel.
2. the preparation method of a kind of cellular globular powdered nickel according to claim 1 is characterized in that described soluble nickel salt is a kind of in nickelous sulfate, nickel chloride or the nickel nitrate.
3. the preparation method of a kind of cellular globular powdered nickel according to claim 1; It is characterized in that it is 50～70g/L that described soluble nickel salting liquid and ammonium oxalate solution carry out course of reaction nickel salt solution concentration, the volumetric concentration of ammonium oxalate solution is 40～60%, logical liquefied ammonia regulator solution pH to 7.5～8.5 during reaction; Under agitation add ammonium oxalate solution; Nickel content≤0.5g/L is terminal point in supernatant, and filtration washing obtains spherical nickel oxalate product after the drying.
4. the preparation method of a kind of cellular globular powdered nickel according to claim 1 is characterized in that under the situation of 300-450 ℃ of also logical hydrogen, carrying out reductase 12-3h to the spherical nickel oxalate that makes, and obtains the cellular globular powdered nickel after the cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100870072A CN102601379A (en) | 2012-03-29 | 2012-03-29 | Method for preparing porous spherical nickel powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100870072A CN102601379A (en) | 2012-03-29 | 2012-03-29 | Method for preparing porous spherical nickel powder |
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| CN102601379A true CN102601379A (en) | 2012-07-25 |
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| CN2012100870072A Pending CN102601379A (en) | 2012-03-29 | 2012-03-29 | Method for preparing porous spherical nickel powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
| CN106180745A (en) * | 2016-08-31 | 2016-12-07 | 昆山德泰新材料科技有限公司 | A kind of foam copper powder and preparation method thereof |
| CN108907229A (en) * | 2018-07-24 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of ellipsoid porous hollow nickel powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11335709A (en) * | 1998-05-21 | 1999-12-07 | Sakai Chem Ind Co Ltd | Production of fine spherical powder of metal nickel |
| EP1160033A1 (en) * | 1999-11-19 | 2001-12-05 | Sakai Chemical Industrial Company Ltd. | Method for producing fine powder of metallic nickel comprised of fine spherical particles |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN101837464A (en) * | 2009-08-28 | 2010-09-22 | 上海九鼎粉体材料有限公司 | Metal nickel powder and preparation method thereof |
-
2012
- 2012-03-29 CN CN2012100870072A patent/CN102601379A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11335709A (en) * | 1998-05-21 | 1999-12-07 | Sakai Chem Ind Co Ltd | Production of fine spherical powder of metal nickel |
| EP1160033A1 (en) * | 1999-11-19 | 2001-12-05 | Sakai Chemical Industrial Company Ltd. | Method for producing fine powder of metallic nickel comprised of fine spherical particles |
| EP1160033A4 (en) * | 1999-11-19 | 2004-05-12 | Sakai Chemical Industry Co | Method for producing fine powder of metallic nickel comprised of fine spherical particles |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN101837464A (en) * | 2009-08-28 | 2010-09-22 | 上海九鼎粉体材料有限公司 | Metal nickel powder and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
| CN106180745A (en) * | 2016-08-31 | 2016-12-07 | 昆山德泰新材料科技有限公司 | A kind of foam copper powder and preparation method thereof |
| CN106180745B (en) * | 2016-08-31 | 2018-07-27 | 昆山德泰新材料科技有限公司 | A kind of foam copper powder and preparation method thereof |
| CN108907229A (en) * | 2018-07-24 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of ellipsoid porous hollow nickel powder |
| CN108907229B (en) * | 2018-07-24 | 2021-08-27 | 安徽工业大学 | Preparation method of ellipsoidal porous hollow nickel powder |
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Application publication date: 20120725 |