CN1600480A - Method for preparing powder of fibroid nickel powder and powder of nickelous oxide - Google Patents
Method for preparing powder of fibroid nickel powder and powder of nickelous oxide Download PDFInfo
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- CN1600480A CN1600480A CN 03159577 CN03159577A CN1600480A CN 1600480 A CN1600480 A CN 1600480A CN 03159577 CN03159577 CN 03159577 CN 03159577 A CN03159577 A CN 03159577A CN 1600480 A CN1600480 A CN 1600480A
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Abstract
A process for preparing the fibrous Ni powder and nickelous oxide powder features that the deposit-transforming thermodecomposing method is used, which includes synthesizing the deposit of their precursor in Ni-NH3-NH4-SG-C2O4-H2O system and the precursor is thermally decomposed in oxidizing atmosphere to obtain to obtain fibrous nickelous oxide powder or in non-oxidizing atmopshere to obtain fibrous Ni powder.
Description
Technical field:
The present invention relates to a kind of preparation technology of extraordinary powder functional materials, the preparation method of especially fibrous nickel powder and nickel protoxide powder.
Background technology:
Special Nickel Powder demonstrates many exceptional functions owing to have great volume effect, surface effects and shape characteristic in fields such as catalyzer, battery material, electrocondution slurry, electromagnetic wave absorbent material, millipore filtration modulator material, powder metallurgy.As a kind of type material, more and more receive publicity, its purposes is wide, and demand is big.The Special Nickel Powder of using mainly adopts carbonyl process production at present.This method is to carry out under High Temperature High Pressure, and nickle carbonoxide is inflammable, explosive, poisonous, contaminate environment, and the process control complexity, and product granularity can only reach micron order, and range of application is limited.Though disclose a kind of method for preparing needle-like or fibrous nickel powder among the Japanese Patent JP64-28309, the presoma of this method is synthetic to be to carry out in autoclave, and its treatment capacity is limited, and requires High Temperature High Pressure, cost height, complicated operation.
Nickel protoxide is a kind of up-and-coming important inorganic materials, and it is widely used in aspects such as catalystic material, battery material, magneticsubstance, electronic material, glass, enamel, stupalith.At present both at home and abroad the preparation method of nickel protoxide powder generally is that carbonate, nitrate or oxyhydroxide with nickel are raw material, get through calcining, and also having with the nickelous chloride is raw material, adds ammonium oxalate and generates nickelous oxalate and precipitate, and calcines in air and gets; Foreign matter content is higher in the product that these methods obtain, and coarse size does not have fibrous shape characteristic again.In addition, preparation nickel protoxide powder also has some additive methods, but the overwhelming majority focuses on spherical nickel protoxide of preparation or nanometer film in these methods, and the report of fibrous nickel protoxide powder is seldom arranged.
Summary of the invention:
The objective of the invention is to overcome the weak point of aforesaid method, the preparation method of a kind of fibrous nickel powder and nickel protoxide powder is provided.This method is safe and reliable, and nontoxic pollution-free is environmentally friendly; Adopt flow process one covering device, just can obtain two kinds of superfine powdery materials as long as change pyrolysated atmosphere, and be easy to realize industrialization; The nickel powder purity height of wherein preparing, granularity is little, specific surface area is big, oxidation-resistance is strong, can satisfy the requirement of domestic and international many fields to nickel powder.
Technical scheme of the present invention: sedimentary pattern of control and granularity in solution, under certain temperature and atmosphere regulation and control, the exsiccant throw out is carried out thermolysis subsequently, obtain the metal and the oxide powder thereof of required pattern and granularity.
The preparation method of fibrous nickel powder is characterized in that: at first add in the reactor, at Ni with certain feed way with the soluble nickel salts solution with by stoichiometric composite precipitation agent solution
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2O (SG
N-Represent acid group Cl
-, SO
4 2-, CH
3COO
-Perhaps NO
3 -) carry out composite precipitation in the system and transform, controlled temperature is 55～85 ℃, pH is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is nickel powder; The electric furnace that subsequently powdered nickel precursor body is placed PID to regulate, controlled temperature is 350～650 ℃, and carries out thermolysis under the non-oxidizing atmosphere regulation and control; Nickel powder after thermolysis finished cools off immediately and surface anti-oxidation is handled, and obtains fibrous nickel powder.
The preparation method of fibrous nickel protoxide powder is characterized in that: at first add in the reactor, at Ni with certain feed way through feeding device with the soluble nickel salts solution and by stoichiometric composite precipitation agent solution
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2O (SG
N-Represent acid group Cl
-, SO
4 2-, CH
3COO
-Perhaps NO
3 -) carry out composite precipitation in the system and transform, controlled temperature is 55～85 ℃, PH is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is the nickel protoxide powder; And then the presoma of nickel protoxide is placed the electric furnace of PID adjusting, controlled temperature is 350～800 ℃, and carries out thermolysis under the oxidizing atmosphere regulation and control; The direct cooling of nickel protoxide powder after thermolysis finished promptly obtains fibrous nickel protoxide powder.
Said soluble nickel salt comprises six water nickelous chlorides among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder, nickel sulfate hexahydrate, four water acetic acid nickel, six water nickelous nitrate or nickel chloride solutions, nickel sulfate solution, nickel acetate solution, nickel nitrate solution.
Compound precipitants described in the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder comprises oxalic acid, oxalate, ammoniacal liquor, alkali and dispersion agent PVP.
Said stoichiometric coefficient by stoichiometric compound precipitants is 1.0～2.0 among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder.
Among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder, the pH value is regulated with ammoniacal liquor, and control ammonia nickel ratio is 2.0～10.0.
Said oxidizing atmosphere comprises oxygen and air atmosphere among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder, and said non-oxidizing atmosphere comprises that hydrogen, hydrogen add nitrogen, hydrogen adds rare gas element and pure inert gas atmosphere.
Said surface anti-oxidation processing method is the carbon dioxide absorption method under the temperature adjusting among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder.
The present invention has the following advantages:
1. adopt precipitation transition heat decomposition method, Ni at normal temperatures and pressures
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2O (SG
N-Represent acid group Cl
-, SO
4 2-, NO
3 -Or CH
3COO
-) carry out nickel powder or nickel protoxide powder presoma building-up process in the system, and follow-up safe and reliable, the nontoxic pollution-free of presoma thermal decomposition process, environmentally friendly.
2. it is to carry out in the same set of device under temperature and atmosphere regulation and control that the fibrous nickel powder surface anti-oxidation after thermolysis is finished is handled.
3, nickel powder and the nickel protoxide powder produced according to the present invention are fibrous, granularity be nano level, porous, specific surface area greatly, wherein the nickel powder anti-aging capability is strong; And fibrous nickel protoxide powder can also obtain globular nickel protoxide powder through after the fine grinding; These powders all can satisfy multi-purpose requirement.
Description of drawings:
Fig. 1: preparation technology's schema of fibrous nickel powder and nickel protoxide powder among the present invention
Fig. 2: the presoma XRD figure of fibrous nickel powder or nickel protoxide powder among the present invention
Fig. 3: the XRD figure of fibrous nickel powder among the present invention
Fig. 4: the XRD figure of fibrous nickel protoxide powder among the present invention
Fig. 5: the presoma SEM of fibrous nickel powder or nickel protoxide powder figure among the present invention
Fig. 6: the SEM of fibrous nickel powder figure among the present invention
Fig. 7: the SEM of fibrous nickel protoxide powder figure among the present invention
Fig. 8: the SEM figure after fibrous nickel protoxide powder grinds among the present invention
Fig. 1 has described the preparation process of fibrous nickel powder and nickel protoxide powder:
1. soluble nickel salts solution and composite precipitation agent solution are added reactor respectively through feeding device, at Ni
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2O (SG
N-Represent acid group Cl
-, SO
4 2-, NO
3 -Or CH
3COO
-) carrying out the composite precipitation conversion reaction in the system, controlled temperature is 55～85 ℃, pH is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l;
2. the composite precipitation thing that obtains after reaction being finished is nickel powder or nickel protoxide powder presoma through washing, filtration and drying;
3. presoma is inserted in the electric furnace of PID adjusting, controlled temperature is 350～650 ℃, carries out thermolysis under the non-oxidizing atmosphere regulation and control; In same set of device, cool off with surface anti-oxidation immediately and handle, obtain fibrous nickel powder to room temperature;
4. presoma is inserted in the electric furnace of PID adjusting, controlled temperature is 350～800 ℃, carries out thermolysis under the oxidizing atmosphere regulation and control, obtains fibrous nickel protoxide powder;
After testing, its physicochemical property is as follows:
Fibrous nickel powder:
Granularity: minor axis≤100nm; Major diameter: 〉=10 μ m; Specific surface area: 〉=13m
2/ g;
Carbon :≤0.01wt%; Sulphur :≤0.001wt%; Iron :≤0.01wt%; Oxygen :≤0.15wt%
Fibrous nickel protoxide powder:
Granularity: minor axis≤150nm; Major diameter: 〉=10 μ m; Specific surface area: 〉=10m
2/ g;
Carbon :≤0.01wt%; Sulphur :≤0.001wt%; Iron :≤0.01wt%;
Embodiment:
Embodiment 1:
Nickel chloride solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-Cl
--C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is about 60 ℃, and regulating pH with ammoniacal liquor is about 8.5, initial Ni in the feed liquid
2+Concentration is 0.8mol/l, C
2O
4 2-Concentration is 0.88mol/l.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, controlled temperature is about 450 ℃, and at (H
2+ N
2) atmosphere regulation and control under carry out thermolysis.Cool off under carbon dioxide atmosphere with surface anti-oxidation immediately after thermolysis is finished and handle to room temperature, the dark gray powder that take out from burn boat the back of coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 2:
Nickel nitrate solution and the composite precipitation agent solution be made up of ammonia, sodium oxalate and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-NO
3 -C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is about 65 ℃, and pH is about 8.6, initial Ni in the feed liquid
2+Concentration is 0.6mol/l, C
2O
4 2-Concentration is 0.72mol/l.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, controlled temperature is about 400 ℃, and at N
2Atmosphere regulation and control carry out thermolysis down, under carbon dioxide atmosphere, cool off with surface anti-oxidation immediately after thermolysis is finished and handle to room temperature, the dark gray powder that take out from the burning boat back of coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 3:
Nickel sulfate solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-SO
4 2--C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is 70 ℃, and pH is 8.8, initial Ni in the feed liquid
2+Concentration is 0.5mol/l, C
2O
4 2-Concentration is 0.65mol/l.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, controlled temperature is 360 ℃, and at (H
2+ N
2) atmosphere regulation and control under carry out thermolysis, under carbon dioxide atmosphere, cool off immediately after thermolysis is finished and handle to room temperature with surface anti-oxidation.The dark gray powder of taking out from burn boat after coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 4:
Nickel acetate solution and the composite precipitation agent solution be made up of ammonia, oxalic acid and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-CH
3COO
--C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is 65 ℃, and pH is 8.7, initial Ni in the feed liquid
2+Concentration is 0.7mol/l, C
2O
4 2-Concentration is 0.85mol/l.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, controlled temperature is 420 ℃, and at N
2Atmosphere regulation and control carry out thermolysis down, under carbon dioxide atmosphere, cool off with surface anti-oxidation immediately after thermolysis is finished and handle to room temperature, the dark gray powder that take out from the burning boat back of coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 5:
Nickel chloride solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-Cl
--C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is about 60 ℃, and regulating pH with ammoniacal liquor is about 8.5, initial Ni in the feed liquid
2+Concentration is 0.8mol/l, C
2O
4 2-Concentration is 0.88mol/l.
After reaction is finished the composite precipitation thing that obtains is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, controlled temperature is 400 ℃, and under air atmosphere, carry out thermolysis, be cooled to room temperature after thermolysis is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Embodiment 6:
Nickel nitrate solution and the composite precipitation agent solution be made up of ammonia, sodium oxalate and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is about 65 ℃, and pH is about 8.6, initial Ni in the feed liquid
2+Concentration is 0.6mol/l, C
2O
4 2-Concentration is 0.72mol/l.
After reaction is finished the composite precipitation thing that obtains is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, controlled temperature is 450 ℃, under oxygen atmosphere, carry out thermolysis, be cooled to room temperature after thermolysis is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Embodiment 7:
Nickel sulfate solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-SO
4 2--C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is 70 ℃, and pH is 8.8, initial Ni in the feed liquid
2+Concentration is 0.5mol/l, C
2O
4 2-Concentration is 0.65mol/l.
After reaction is finished the composite precipitation thing that obtains is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, controlled temperature is 500 ℃, under air atmosphere, carry out thermolysis, be cooled to room temperature after thermolysis is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Embodiment 8:
Nickel acetate solution and the composite precipitation agent solution be made up of ammonia, oxalic acid and dispersion agent PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-CH
3COO
--C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, controlled temperature is 65 ℃, and pH is 8.7, initial Ni in the feed liquid
2+Concentration is 0.7mol/l, C
2O
4 2-Concentration is 0.85mol/l.
After reaction is finished the composite precipitation thing that obtains is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, controlled temperature is 650 ℃, under oxygen atmosphere, carry out thermolysis, be cooled to room temperature after thermolysis is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Claims (8)
1. the preparation method of fibrous nickel powder is characterized in that: at first add in the reactor, at Ni with certain feed way through feeding device with the soluble nickel salts solution and by stoichiometric composite precipitation agent solution
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2O (SG
N-Represent acid group Cl
-, SO
4 2-, CH
3COO
-Perhaps NO
3 -) carry out composite precipitation in the system and transform, controlled temperature is 55～85 ℃, PH is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is nickel powder; And then the presoma of nickel powder is placed the electric furnace of PID adjusting, controlled temperature is 350～650 ℃, carries out thermolysis under the non-oxidizing atmosphere regulation and control, and the nickel powder after thermolysis is finished cools off immediately and surface anti-oxidation is handled, and obtains fibrous nickel powder.
2. the preparation method of fibrous nickel protoxide powder is characterized in that: at first add in the reactor, at Ni with certain feed way through feeding device with the soluble nickel salts solution and by stoichiometric composite precipitation agent solution
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2O (SG
N-Represent acid group Cl
-, SO
4 2-, CH
3COO
-Perhaps NO
3 -) carry out composite precipitation in the system and transform, controlled temperature is 55～85 ℃, PH is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is the nickel protoxide powder; And then the presoma of nickel protoxide is placed the electric furnace of PID adjusting, controlled temperature is 350～800 ℃, and carries out thermolysis under the oxidizing atmosphere regulation and control, and the direct cooling of nickel oxide powder after thermolysis is finished promptly obtains fibrous nickel protoxide powder.
3. according to claim 1,2 described methods, it is characterized in that described soluble nickel salt comprises six water nickelous chlorides, nickel sulfate hexahydrate, four water acetic acid nickel, six water nickelous nitrate or nickel chloride solutions, nickel sulfate solution, nickel acetate solution, nickel nitrate solution.
4. according to claim 1,2 described methods, it is characterized in that described compound precipitants comprises oxalic acid, oxalate, ammoniacal liquor, alkali and dispersion agent PVP.
5. according to claim 1,2 described methods, it is characterized in that described stoichiometric coefficient by stoichiometric compound precipitants is 1.0～2.0.
6. according to claim 1,2 described methods, it is characterized in that regulating the pH value with ammoniacal liquor, control ammonia nickel ratio is 2.0～10.0.
7. according to claim 1,2 described methods, it is characterized in that described oxidizing atmosphere comprises oxygen atmosphere and air atmosphere, described non-oxidizing atmosphere comprises that hydrogen, hydrogen add nitrogen, hydrogen adds rare gas element and pure inert gas atmosphere.
8. according to claim 1,2 described methods, it is characterized in that described surface anti-oxidation processing method is meant the carbon dioxide absorption method under the temperature adjusting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031595774A CN1299866C (en) | 2003-09-24 | 2003-09-24 | Method for preparing powder of fibroid nickel powder and powder of nickelous oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031595774A CN1299866C (en) | 2003-09-24 | 2003-09-24 | Method for preparing powder of fibroid nickel powder and powder of nickelous oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1600480A true CN1600480A (en) | 2005-03-30 |
| CN1299866C CN1299866C (en) | 2007-02-14 |
Family
ID=34660690
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103464784A (en) * | 2013-09-27 | 2013-12-25 | 南开大学 | Preparation method of nano nickel supported on carbon |
| CN103498071A (en) * | 2013-09-18 | 2014-01-08 | 中南大学 | Preparation method of porous copper-nickel alloy fiber |
| CN109134235A (en) * | 2018-09-17 | 2019-01-04 | 郑州工程技术学院 | A kind of preparation method of the complicated oxalic acid nickel salt of threadiness |
| CN109369380A (en) * | 2018-11-23 | 2019-02-22 | 中南大学 | A method of fine shape is prepared by recrystallization and ties up oxalic acid nickel powder, fibrous nickel powder and fibrous nickel protoxide powder |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1423285A1 (en) * | 1987-01-09 | 1988-09-15 | Научно-исследовательский институт физико-химических проблем Белорусского государственного университета им.В.И.Ленина | Method of producing nickel powder |
| JPH0745684B2 (en) * | 1987-07-23 | 1995-05-17 | 住友金属鉱山株式会社 | Nickel fine powder manufacturing method |
| US5130204A (en) * | 1988-02-11 | 1992-07-14 | Jenkin William C | Randomly dispersed metal fiber mat |
| CN1074946A (en) * | 1992-01-31 | 1993-08-04 | 孟宇 | Refine the processing method of nickel oxide from the aluminium scrap nickel alloy powder |
| JP3479814B2 (en) * | 1994-07-27 | 2003-12-15 | 太平化学産業株式会社 | How to collect valuables |
-
2003
- 2003-09-24 CN CNB031595774A patent/CN1299866C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103498071A (en) * | 2013-09-18 | 2014-01-08 | 中南大学 | Preparation method of porous copper-nickel alloy fiber |
| CN103498071B (en) * | 2013-09-18 | 2015-06-17 | 中南大学 | Preparation method of porous copper-nickel alloy fiber |
| CN103464784A (en) * | 2013-09-27 | 2013-12-25 | 南开大学 | Preparation method of nano nickel supported on carbon |
| CN103464784B (en) * | 2013-09-27 | 2016-01-20 | 南开大学 | A kind of preparation method of carbon loaded with nano nickel |
| CN109134235A (en) * | 2018-09-17 | 2019-01-04 | 郑州工程技术学院 | A kind of preparation method of the complicated oxalic acid nickel salt of threadiness |
| CN109369380A (en) * | 2018-11-23 | 2019-02-22 | 中南大学 | A method of fine shape is prepared by recrystallization and ties up oxalic acid nickel powder, fibrous nickel powder and fibrous nickel protoxide powder |
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| Publication number | Publication date |
|---|---|
| CN1299866C (en) | 2007-02-14 |
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