CN102616866A - Preparation method of porous spherical nickel oxide powder - Google Patents
Preparation method of porous spherical nickel oxide powder Download PDFInfo
- Publication number
- CN102616866A CN102616866A CN2012100870068A CN201210087006A CN102616866A CN 102616866 A CN102616866 A CN 102616866A CN 2012100870068 A CN2012100870068 A CN 2012100870068A CN 201210087006 A CN201210087006 A CN 201210087006A CN 102616866 A CN102616866 A CN 102616866A
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- China
- Prior art keywords
- spherical
- oxide powder
- preparation
- vesicular
- nickel oxide
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- 239000000843 powder Substances 0.000 title claims abstract description 37
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 29
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 34
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000002815 nickel Chemical class 0.000 claims abstract description 16
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 22
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- LVIYYTJTOKJJOC-UHFFFAOYSA-N nickel phthalocyanine Chemical compound [Ni+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 LVIYYTJTOKJJOC-UHFFFAOYSA-N 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- XVENFWPVABIFLP-UHFFFAOYSA-N nickel;oxalic acid Chemical compound [Ni].OC(=O)C(O)=O XVENFWPVABIFLP-UHFFFAOYSA-N 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 abstract 2
- 238000005272 metallurgy Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 210000003298 dental enamel Anatomy 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000005320 cranberry glass Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of porous spherical nickel oxide powder and relates to the preparation method of the porous spherical nickel oxide powder in wet metallurgy. The preparation method is characterized in that in the preparation process, soluble nickel salt solution reacts with ammonium oxalate solution to obtain spherical nickel oxalate, then, the prepared spherical nickel oxalate is calcined, and the porous spherical nickel oxide powder is prepared. The preparation method of the porous spherical nickel oxide powder provided by the invention has the advantages that the powder body of the prepared spherical nickel oxide powder is in a spherical shape, in addition, the surface is in a porous shape, the specific surface area is large, and the requirements of special industries can be met.
Description
Technical field
The preparation method of the spherical nickel oxide powder of a kind of vesicular relates to the preparation method of the spherical nickel oxide powder of vesicular in a kind of hydrometallurgy.
Background technology
Nickel protoxide is mainly used in the adhesive agent and the tinting material of enamel, ceramic industry enamel, one of main constitutive material in the nickel-zinc ferrite magneticsubstance.Glass industry is as the tinting material of cranberry glass and picture tube glass bulb.It also is the raw material of making nickel salt and nickel catalyzator.Also be used for store battery, the additive of industries such as electronic industry, for example semi-conductor air-sensitive material, fuel cell electrode material, electrode material for super capacitor, corrosion protection coating etc.In recent years, along with the fast development of electronic industry especially ultracapacitor, the application prospect of nickel protoxide is boundless.
Through consulting reference materials, at present, the preparation method of the spherical nickel oxide powder of vesicular does not also report.
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 powder spherical in shape, and the surface is vesicular, specific surface area is big, can satisfy the special industry demand.
The objective of the invention is to realize through following technical scheme.
The preparation method of the spherical nickel oxide powder of a kind of vesicular; It is characterized in that its its process of preparation is with soluble nickel salts solution and ammonium oxalate solution reaction; Obtain spherical nickelous oxalate, calcine the spherical nickelous oxalate that makes then, make the spherical nickel oxide powder of vesicular.
The preparation method of the spherical nickel oxide powder of a kind of vesicular of the present invention is characterized in that described soluble nickel salt is a kind of in single nickel salt, nickelous chloride or the nickelous nitrate.
The preparation method of the spherical nickel oxide powder of a kind of vesicular of the present invention; It is characterized in that described soluble nickel salts solution and ammonium oxalate solution reaction process, the degree of depth of nickel salt solution is 50～70g/L, and the weight ratio degree of depth of ammonium oxalate solution is 40%～60% solution; Temperature of reaction is 40～60 ℃; Logical liquefied ammonia regulator solution pH to 7.5～8.5 under agitation add ammonium oxalate solution, and nickel content≤0.5g/L is terminal point in supernatant; Filtration washing obtains the spherical oxalic acid nickel powder of vesicular after the drying.
The preparation method of the spherical nickel oxide powder of a kind of vesicular of the present invention is characterized in that it is at 400-500 ℃ of calcining 2-3h that spherical nickelous oxalate that described handle makes carries out calcination process, obtains the spherical nickel oxide powder of vesicular after the cooling.
The preparation method of the spherical nickel oxide powder of a kind of vesicular of the present invention, the spherical nickel oxide powder that makes, not only powder is spherical in shape, and the surface is vesicular, and specific surface area is big, can satisfy the special industry demand.
Embodiment
The preparation method of the spherical nickel oxide powder of a kind of vesicular, its its process of preparation are with soluble nickel salts solution and ammonium oxalate solution reaction, obtain spherical nickelous oxalate, calcine the spherical nickelous oxalate that makes then, make the spherical nickel oxide powder of vesicular.
Embodiment 1
The concentration that with the single nickel salt is the preparation of raw material nickel solution is 50.33g/L; The weight ratio concentration of ammonium oxalate solution is 40% solution, and temperature of reaction is 40 ℃, logical liquefied ammonia regulator solution pH to 7.5; Under agitation add ammonium oxalate solution; Nickel content≤0.5g/L is terminal point in supernatant, and filtration washing obtains the spherical oxalic acid nickel powder of vesicular after the drying; Carrying out calcination process to the spherical nickelous oxalate that makes is at 400 ℃ of about 2h of calcining, obtains the spherical nickel oxide powder of vesicular after the cooling.
Embodiment 2
The concentration that with the single nickel salt is the preparation of raw material nickel solution is 59.87g/L,, the weight ratio concentration of ammonium oxalate solution is 50% solution; Temperature of reaction is 50 ℃; Logical liquefied ammonia regulator solution pH to 8 under agitation adds ammonium oxalate solution, and nickel content≤0.5g/L is terminal point in supernatant; Filtration washing obtains the spherical oxalic acid nickel powder of vesicular after the drying; Carrying out calcination process to the spherical nickelous oxalate that makes is at 450 ℃ of about 2.5h of calcining, obtains the spherical nickel oxide powder of vesicular after the cooling.
Embodiment 3
The concentration that with the single nickel salt is the preparation of raw material nickel solution is 69.13g/L,, the weight ratio concentration of ammonium oxalate solution is 60% solution; Temperature of reaction is 60 ℃; Logical liquefied ammonia regulator solution pH to 8.5 under agitation adds ammonium oxalate solution, and nickel content≤0.5g/L is terminal point in supernatant; Filtration washing obtains the spherical oxalic acid nickel powder of vesicular after the drying; Carrying out calcination process to the spherical nickelous oxalate that makes is at 500 ℃ of about 3h of calcining, obtains the spherical nickel oxide powder of vesicular after the cooling.
Claims (4)
1. the preparation method of the spherical nickel oxide powder of a vesicular; It is characterized in that its its process of preparation is with soluble nickel salts solution and ammonium oxalate solution reaction; Obtain spherical nickelous oxalate, calcine the spherical nickelous oxalate that makes then, make the spherical nickel oxide powder of vesicular.
2. the preparation method of the spherical nickel oxide powder of a kind of vesicular according to claim 1 is characterized in that described soluble nickel salt is a kind of in single nickel salt, nickelous chloride or the nickelous nitrate.
3. the preparation method of the spherical nickel oxide powder of a kind of vesicular according to claim 1; It is characterized in that described soluble nickel salts solution and ammonium oxalate solution reaction process, the degree of depth of nickel salt solution is 50～70g/L, and the weight ratio degree of depth of ammonium oxalate solution is 40%～60% solution; Temperature of reaction is 40～60 ℃; Logical liquefied ammonia regulator solution pH to 7.5～8.5 under agitation add ammonium oxalate solution, and nickel content≤0.5g/L is terminal point in supernatant; Filtration washing obtains the spherical oxalic acid nickel powder of vesicular after the drying.
4. the preparation method of the spherical nickel oxide powder of a kind of vesicular according to claim 1 is characterized in that it is at 400-500 ℃ of calcining 2-3h that spherical nickelous oxalate that described handle makes carries out calcination process, obtains the spherical nickel oxide powder of vesicular after the cooling.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100870068A CN102616866A (en) | 2012-03-29 | 2012-03-29 | Preparation method of porous spherical nickel oxide powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100870068A CN102616866A (en) | 2012-03-29 | 2012-03-29 | Preparation method of porous spherical nickel oxide powder |
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| CN102616866A true CN102616866A (en) | 2012-08-01 |
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| CN2012100870068A Pending CN102616866A (en) | 2012-03-29 | 2012-03-29 | Preparation method of porous spherical nickel oxide powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923793A (en) * | 2012-11-15 | 2013-02-13 | 宿迁学院 | Method for preparing nanometer nickel oxide |
| CN108706640A (en) * | 2018-07-13 | 2018-10-26 | 金川集团股份有限公司 | A kind of preparation method of nickel oxide powder material |
| CN112897598A (en) * | 2021-02-07 | 2021-06-04 | 阳江市联邦金属化工有限公司 | Preparation method of superfine nickel protoxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1114639A (en) * | 1994-07-02 | 1996-01-10 | 雷慧绪 | Method for producing cobalt oxide nickel oxide powder for electronic industry |
| JP2004315274A (en) * | 2003-04-15 | 2004-11-11 | Sumitomo Metal Mining Co Ltd | Acicular nickel oxide powder and its manufacturing method |
| CN102070209A (en) * | 2010-12-14 | 2011-05-25 | 荆门市格林美新材料有限公司 | Method for synthesizing nickel oxide precursor by multi-step precipitation and preparation method of nickel oxide |
-
2012
- 2012-03-29 CN CN2012100870068A patent/CN102616866A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1114639A (en) * | 1994-07-02 | 1996-01-10 | 雷慧绪 | Method for producing cobalt oxide nickel oxide powder for electronic industry |
| JP2004315274A (en) * | 2003-04-15 | 2004-11-11 | Sumitomo Metal Mining Co Ltd | Acicular nickel oxide powder and its manufacturing method |
| CN102070209A (en) * | 2010-12-14 | 2011-05-25 | 荆门市格林美新材料有限公司 | Method for synthesizing nickel oxide precursor by multi-step precipitation and preparation method of nickel oxide |
Non-Patent Citations (2)
| Title |
|---|
| 傅小明 等: "空气中热分解二水草酸镍制备纳米氧化镍", 《中国有色冶金》 * |
| 李文选 等: "草酸镍的制备与研究", 《中国有色冶金》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923793A (en) * | 2012-11-15 | 2013-02-13 | 宿迁学院 | Method for preparing nanometer nickel oxide |
| CN108706640A (en) * | 2018-07-13 | 2018-10-26 | 金川集团股份有限公司 | A kind of preparation method of nickel oxide powder material |
| CN112897598A (en) * | 2021-02-07 | 2021-06-04 | 阳江市联邦金属化工有限公司 | Preparation method of superfine nickel protoxide |
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Application publication date: 20120801 |