CN102709529B - Method for enhancing properties of spherical nickel hydroxide - Google Patents
Method for enhancing properties of spherical nickel hydroxide Download PDFInfo
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- CN102709529B CN102709529B CN201210137691.0A CN201210137691A CN102709529B CN 102709529 B CN102709529 B CN 102709529B CN 201210137691 A CN201210137691 A CN 201210137691A CN 102709529 B CN102709529 B CN 102709529B
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- nickel hydroxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a method for enhancing properties of spherical nickel hydroxide, which is characterized in that mixed rare-earth components are added in the spherical nickel hydroxide preparation process, wherein the mixed rare-earth components account for 0.1-1.5 wt% of the spherical nickel hydroxide. The active substance of the nickel cathode using the spherical nickel hydroxide has high electrochemical activity, and high bulk density to enhance the volume ratio capacity of the nickel electrode; and the battery has the advantages of small size, light weight, high capacity and long service life.
Description
Technical field
The present invention relates to a kind of method that improves ball-shape nickel hydroxide performance, particularly a kind of method that improves ball-shape nickel hydroxide tap density and gram specific capacity.
Background technology
Along with portable communication apparatus and portable electronics developing rapidly and universal, people constantly propose requirements at the higher level to the energy density of secondary cell, volume is little, lightweight, capacity is high and the demand of the alkaline secondary cell that the life-span is long sharply increases.Ball-shape nickel hydroxide is as the active material of nickel positive pole, and its electrical property directly has influence on battery performance.Therefore, for adapting to the needs of nickel-based battery development, ball-shape nickel hydroxide not only will have high electro-chemical activity, and will have high bulk density to improve the volume and capacity ratio of nickel electrode.
The general ball-shape nickel hydroxide basic product standard of the He Qiu of current battery manufacturer nickel manufacturer is:
| Project | Add Cd index | Zn3.0 index | Zn4.0 index | Zn4.5 index |
| Apparent density, g/cm 3 | ≥1.65 | ≥1.65 | ≥1.65 | ≥1.65 |
| Tap density, g/cm 3 | ≥2.10 | ≥2.10 | ≥2.10 | ≥2.10 |
| Granularity D50, ц m | 9--14 | 7--12 | 7--12 | 7--12 |
| Specific area, m 2/g | 9.0--25.0 | 5.0--15.0 | 5.0--15.0 | 5.0--15.0 |
| 101 diffraction maximum half-peak breadths, deg | 0.67--0.75 | 0.67--0.75 | 0.67--0.75 | 0.67--0.75 |
| Ni+Co，% | ≥58.5 | ≥58 | ≥58 | ≥55.5 |
| Co，% | ≥0.90 | 1.3--1.7 | ≥1.30 | ≥0.60 |
| Cd，% | 2.9--3.5 | ≤0.002 | ≤0.002 | |
| Zn，% | 2.8--3.2 | 3.7--4.3 | 4.1--4.9 | |
| Fe，% | ≤0.01 | ≤0.01 | ≤0.01 | ≤0.01 |
| Mn，% | ≤0.01 | ≤0.01 | ≤0.01 | ≤0.01 |
| Mg，% | ≤0.05 | ≤0.05 | ≤0.05 | ≤0.05 |
| Cu，% | ≤0.01 | ≤0.01 | ≤0.01 | ≤0.01 |
| Ca，% | ≤0.05 | ≤0.05 | ≤0.05 | ≤0.05 |
| Cr，% | ≤0.02 | |||
| Pb，% | ≤0.01 | |||
| SO 4 2-，% | ≤0.3 | ≤0.4 | ≤0.4 | ≤0.4 |
| NO 3 -，% | ≤0.01 | ≤0.01 | ≤0.01 | ≤0.05 |
| Cl -，% | ≤0.01 | ≤0.01 | ≤0.01 | ≤0.05 |
| H 2O，% | ≤1.0 | ≤1.0 | ≤1.5 | ≤1.5 |
| Specific discharge capacity, mAh/g | ≥195 | ≥240 | ≥235 | ≥235 |
Wherein for tap density, require to be>=2.10 g/cm
3, generally can accomplish 2.20～2.25 g/cm
3; Specific discharge capacity requirement, adding cadmium ball nickel is>=195 mAh/g, and adding Zn3.0% is>=240 mAh/g, adds Zn4.0%, adds Zn4.5% and requires as>=235 mAh/g, and common product can reach requirement.Note: the present invention's ball-shape nickel hydroxide specific discharge capacity method of testing used is: ball-shape nickel hydroxide and binding agent PTFE and addition of C MC and cobalt protoxide are mixed, stir into pasty state, evenly be coated on Foamed Nickel matrix, be assembled into battery with excessive hydrogen-storage alloy negative pole, with low current, change into rear charging measurement, charging current is 1C, and discharging current is 1C, is discharged to 1.0V.Tester is new prestige 5V3A battery check device.
The property indices of the ball-shape nickel hydroxide of producing at present, although particularly tap density, specific discharge capacity can reach the requirement of basic product standard, but, owing to being subject to the restriction of each technological parameter in existing preparation technology, but be difficult to further to property indices, particularly tap density, these two crucial performance index of specific discharge capacity are done further to promote, for this reason, the applicant has developed a kind of method that improves ball-shape nickel hydroxide performance, can further improve tap density and the specific discharge capacity of ball-shape nickel hydroxide by the method.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of method that improves ball-shape nickel hydroxide performance, by the method, can effectively improve tap density and the specific discharge capacity of ball-shape nickel hydroxide.
The technical solution adopted for the present invention to solve the technical problems is:
A method that improves ball-shape nickel hydroxide performance, is characterized in that: in ball-shape nickel hydroxide preparation process, add mishmetal composition, the weight of the mishmetal composition of interpolation accounts for 0.1 ~ 1.5% of ball-shape nickel hydroxide total weight.
Above-mentioned mishmetal composition can be the mixing of at least two kinds of rare earth materials in La, Ce, Nd, Pr.
The mode of adding in the process that described mishmetal composition is prepared at ball-shape nickel hydroxide can adopt following technique: by nickel sulfate solution, zinc sulfate solution or the cadmium sulfate aqueous solution, cobalt sulfate solution is made into ball-shape nickel hydroxide feed liquid in the ratio in ball-shape nickel hydroxide technical quality standard, by this feed liquid, ammoniacal liquor, sodium hydrate aqueous solution, mishmetal sulfate liquor is continuously supplied with ball-shape nickel hydroxide reactor with chemical equation ratio, under continuous stirring, control 40 ~ 70 ℃ of solution temperatures, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that has added mishmetal composition, through washing, be dried into finished product.
The invention has the beneficial effects as follows: the ball-shape nickel hydroxide that employing the present invention obtains is as the active material of nickel positive pole, not only there is high electro-chemical activity, and having high bulk density to improve the volume and capacity ratio of nickel electrode, the volume of battery is little, lightweight simultaneously, capacity is high and the life-span is long.
Below in conjunction with embodiment, the present invention is further described.
Embodiment
Embodiment 1
Nickel sulfate solution, the cadmium sulfate aqueous solution, cobalt sulfate solution are pressed to NiSO
41.36mol/L, CoSO
40.026mol/L, CdSO
40.039mol/L is made into mixed liquor, and controls the ZnSO in mixed liquor
4≤ 0.02mol/L, FeSO
4≤ 0.001mol/L, MnSO
4≤ 0.001mol/L, MgSO
4≤ 0.002mol/L, CuSO
4≤ 0.001mol/L, CaSO
4≤ 0.001mol/L, this mixed liquor, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with to ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that does not add mishmetal composition, through washing, be dried into finished product 1.
Then, under above-mentioned identical condition, to contain La, Ce, Nd, the mishmetal sulfate liquor of Pr, the mixed liquor of preparing as stated above, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that has added mishmetal composition, the weight of the mishmetal composition wherein adding accounts for 0.1 ~ 1.5% of ball-shape nickel hydroxide total weight, through washing, be dried into finished product 2.
Finished product 1 and finished product 2 constituent analyses and performance comparison see the following form.
| Project | Finished product 1 | Finished product 2 |
| Mixed rare earth additive | Nothing | Have |
| Apparent density, g/cm 3 | 1.70 | 1.71 |
| Tap density, g/cm 3 | 2.22 | 2.37 |
| Granularity D50, ц m | 10.56 | 10.62 |
| Specific area, m 2/g | 15.62 | 15.83 |
| 101 diffraction maximum half-peak breadths, deg | 0.71 | 0.71 |
| Ni+Co，% | 58.62 | 58.33 |
| Co，% | 1.20 | 1.19 |
| Cd，% | 3.2 | 3.18 |
| Zn，% | 0.35 | 0.34 |
| Fe，% | ≤0.01 | ≤0.01 |
| Mn，% | ≤0.01 | ≤0.01 |
| Mg，% | ≤0.05 | ≤0.05 |
| Cu，% | ≤0.01 | ≤0.01 |
| Ca，% | ≤0.05 | ≤0.05 |
| SO 4 2-，% | ≤0.3 | ≤0.3 |
| NO 3 -，% | ≤0.01 | ≤0.01 |
| Cl -，% | ≤0.01 | ≤0.01 |
| H 2O，% | 0.83 | 0.80 |
| Specific discharge capacity, mAh/g | 202 | 212 |
Embodiment 2
Nickel sulfate solution, zinc sulfate solution, cobalt sulfate solution are pressed to NiSO
41.45mol/L, CoSO
40.038mol/L, ZnSO
40.066mol/L is made into mixed liquor, and controls the CdSO in mixed liquor
4≤ 0.001mol/L, FeSO
4≤ 0.001mol/L, MnSO
4≤ 0.001mol/L, MgSO
4≤ 0.002mol/L, CuSO
4≤ 0.001mol/L, CaSO
4≤ 0.001mol/L, by this mixed liquor, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that does not add mishmetal composition, through washing, be dried into finished product 3.
Then, under above-mentioned identical condition, to contain La, Ce, Nd, the mishmetal sulfate liquor of Pr, the mixed liquor of preparing as stated above, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that has added mishmetal composition, the weight of the mishmetal composition wherein adding accounts for 0.1 ~ 1.5% of ball-shape nickel hydroxide total weight, through washing, be dried into finished product 4.
Finished product 3 and finished product 4 constituent analyses and performance comparison see the following form.
| Project | Finished product 3 | Finished product 4 |
| Mixed rare earth additive | Nothing | Have |
| Apparent density, g/cm 3 | 1.71 | 1.72 |
| Tap density, g/cm 3 | 2.25 | 2.38 |
| Granularity D50, ц m | 9.58 | 9.64 |
| Specific area, m 2/g | 12.31 | 11.69 |
| 101 diffraction maximum half-peak breadths, deg | 0.69 | 0.72 |
| Ni+Co，% | 58.32 | 58.03 |
| Co，% | 1.52 | 1.51 |
| Cd，% | ≤0.002 | ≤0.002 |
| Zn，% | 3.02 | 3.00 |
| Fe，% | ≤0.01 | ≤0.01 |
| Mn，% | ≤0.01 | ≤0.01 |
| Mg，% | ≤0.05 | ≤0.05 |
| Cu，% | ≤0.01 | ≤0.01 |
| Ca，% | ≤0.05 | ≤0.05 |
| SO 4 2-，% | ≤0.3 | ≤0.3 |
| NO 3 -，% | ≤0.01 | ≤0.01 |
| Cl -，% | ≤0.01 | ≤0.01 |
| H 2O，% | 0.76 | 0.79 |
| Specific discharge capacity, mAh/g | 241 | 249 |
Embodiment 3
Nickel sulfate solution or zinc sulfate solution, cobalt sulfate solution are pressed to NiSO
41.53mol/L, CoSO
40.041mol/L, ZnSO
40.095mol/L, and control the CdSO in mixed liquor
4≤ 0.001mol/L, FeSO
4≤ 0.001mol/L, MnSO
4≤ 0.001mol/L, MgSO
4≤ 0.002mol/L, CuSO
4≤ 0.001mol/L, CaSO
4≤ 0.001mol/L, this mixed liquor, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with to ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that does not add mishmetal composition, through washing, be dried into finished product 5.
Then, under above-mentioned identical condition, to contain La, Ce, Nd, the mishmetal sulfate liquor of Pr, the mixed liquor of preparing as stated above, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that has added mishmetal composition, the weight of the mishmetal composition wherein adding accounts for 0.1 ~ 1.5% of ball-shape nickel hydroxide total weight, through washing, be dried into finished product 6.
Finished product 5 and finished product 6 constituent analyses and performance comparison see the following form.
| Project | Finished product 5 | Finished product 6 |
| Mixed rare earth additive | Nothing | Have |
| Apparent density, g/cm 3 | 1.69 | 1.70 |
| Tap density, g/cm 3 | 2.24 | 2.36 |
| Granularity D50, ц m | 9.89 | 9.92 |
| Specific area, m 2/g | 10.69 | 10.73 |
| 101 diffraction maximum half-peak breadths, deg | 0.71 | 0.72 |
| Ni+Co，% | 58.52 | 58.23 |
| Co，% | 1.36 | 1.35 |
| Cd，% | ≤0.002 | ≤0.002 |
| Zn，% | 4.08 | 4.06 |
| Fe，% | ≤0.01 | ≤0.01 |
| Mn，% | ≤0.01 | ≤0.01 |
| Mg，% | ≤0.05 | ≤0.05 |
| Cu，% | ≤0.01 | ≤0.01 |
| Ca，% | ≤0.05 | ≤0.05 |
| SO 4 2-，% | ≤0.3 | ≤0.3 |
| NO 3 -，% | ≤0.01 | ≤0.01 |
| Cl -，% | ≤0.01 | ≤0.01 |
| H 2O，% | 0.91 | 0.89 |
| Specific discharge capacity, mAh/g | 238 | 246 |
Embodiment 4
Nickel sulfate solution or zinc sulfate solution, cobalt sulfate solution are pressed to NiSO
41.62mol/L, CoSO
40.048mol/L, ZnSO
40.113mol/L, is made into mixed liquor, and controls the CdSO in mixed liquor
4≤ 0.001mol/L, FeSO
4≤ 0.001mol/L, MnSO
4≤ 0.001mol/L, MgSO
4≤ 0.002mol/L, CuSO
4≤ 0.001mol/L, CaSO
4≤ 0.001mol/L, this mixed liquor, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with to ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that does not add mishmetal composition, through washing, be dried into finished product 7.
Then, under above-mentioned identical condition, under above-mentioned identical condition, to contain La, Ce, Nd, the mishmetal sulfate liquor of Pr, the mixed liquor of preparing as stated above, 1 mol/L ammoniacal liquor, 10 mol/L sodium hydrate aqueous solutions are continuously supplied with ball-shape nickel hydroxide reactor in certain proportion, under strong agitation, controlling 40 ~ 70 ℃ of solution temperatures continuously, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that has added mishmetal composition, the weight of the mishmetal composition wherein adding accounts for 0.1 ~ 1.5% of ball-shape nickel hydroxide total weight, through washing, be dried into finished product 8.
Finished product 5 and finished product 6 constituent analyses and performance comparison see the following form.
| Project | Finished product 7 | Finished product 8 |
| Mixed rare earth additive | Nothing | Have |
| Apparent density, g/cm 3 | 1.72 | 1.73 |
| Tap density, g/cm 3 | 2.25 | 2.39 |
| Granularity D50, ц m | 9.42 | 9.38 |
| Specific area, m 2/g | 9.89 | 9.63 |
| 101 diffraction maximum half-peak breadths, deg | 0.71 | 0.72 |
| Ni+Co，% | 55.63 | 55.35 |
| Co，% | 0.62 | 0.62 |
| Cd，% | ≤0.002 | ≤0.002 |
| Zn，% | 4.53 | 4.51 |
| Fe，% | ≤0.01 | ≤0.01 |
| Mn，% | ≤0.01 | ≤0.01 |
| Mg，% | ≤0.05 | ≤0.05 |
| Cu，% | ≤0.01 | ≤0.01 |
| Ca，% | ≤0.05 | ≤0.05 |
| SO 4 2-，% | ≤0.3 | ≤0.3 |
| NO 3 -，% | ≤0.01 | ≤0.01 |
| Cl -，% | ≤0.01 | ≤0.01 |
| H 2O，% | 0.79 | 0.82 |
| Specific discharge capacity, mAh/g | 239 | 249 |
above-mentioned mixed rare earth solution can also be the mixing of two or three rare earth, the ratio of each component can be: when adopting two components to mix, the content of two components can mix by 1-99%, when adopting three components to mix, the content of three components can mix by 1-98%, when adopting four components to mix, the content of four components can mix by 1-97%.
From above-mentioned example, can draw, the ball-shape nickel hydroxide material tap density of not adding mishmetal composition prepared by similarity condition is (2.20 ~ 2.25) * 10
3kg/m
3, and the ball-shape nickel hydroxide material tap density of having added mishmetal composition can reach (2.35 ~ 2.39) * 10
3kg/m
3.The ball-shape nickel hydroxide material 0.2C electric discharge gram specific capacity of not adding mishmetal composition prepared by similarity condition is for adding cadmium ball-shape nickel hydroxide 195 ~ 202 mAh/g, add Zn3.0% ball-shape nickel hydroxide 240 ~ 245 mAh/g, add Zn4.0% ball-shape nickel hydroxide 235 ~ 240 mAh/g, add Zn4.5% ball-shape nickel hydroxide 235 ~ 240 mAh/g; And the ball-shape nickel hydroxide material 0.2C electric discharge gram specific capacity of having added mishmetal composition is for adding cadmium ball-shape nickel hydroxide 202 ~ 212 mAh/g, add Zn3.0% ball-shape nickel hydroxide 245 ~ 250 mAh/g, add Zn4.0% ball-shape nickel hydroxide 240 ~ 250 mAh/g, add Zn4.5% ball-shape nickel hydroxide 240 ~ 250 mAh/g.
By above-mentioned examples prove, be added with mishmetal composition ball-shape nickel hydroxide as the active material of nickel positive pole, not only have high electro-chemical activity, and have high bulk density to improve the volume and capacity ratio of nickel electrode, the volume of battery is little, lightweight simultaneously, capacity is high and the life-span is long.
Claims (2)
1. a method that improves ball-shape nickel hydroxide performance, it is characterized in that: in ball-shape nickel hydroxide preparation process, add mishmetal composition, the weight of the mishmetal composition adding accounts for 0.1 ~ 1.5% of ball-shape nickel hydroxide total weight, described mishmetal composition is the mixing of two kinds of rare earth materials in La, Ce, Nd, Pr, and in mishmetal composition, the ratio of each rare earth component is: wherein the content of a component is 1-99%, and the content of another component is 99-1%.
2. a kind of method that improves ball-shape nickel hydroxide performance according to claim 1, it is characterized in that: the mode of adding in the process that described mishmetal composition is prepared at ball-shape nickel hydroxide is: by nickel sulfate solution, zinc sulfate solution or the cadmium sulfate aqueous solution, cobalt sulfate solution is made into ball-shape nickel hydroxide feed liquid in the ratio in ball-shape nickel hydroxide technical quality standard, by this feed liquid, ammoniacal liquor, sodium hydrate aqueous solution, mishmetal sulfate liquor is continuously supplied with ball-shape nickel hydroxide reactor with chemical equation ratio, under continuous stirring, control 40 ~ 70 ℃ of solution temperatures, pH 11 ~ 12.5, reaction generates the ball-shape nickel hydroxide that has added mishmetal composition, through washing, be dried into finished product.
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|---|---|---|---|
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|---|---|---|---|
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| CN1129198C (en) * | 1997-02-03 | 2003-11-26 | 松下电器产业株式会社 | Manufacturing method of active materials for positive electrode in alkaline storage batteries |
| JP4341119B2 (en) * | 1999-09-24 | 2009-10-07 | 堺化学工業株式会社 | Method for producing spherical nickel powder |
| WO2003021698A1 (en) * | 2001-09-03 | 2003-03-13 | Yuasa Corporation | Nickel electrode material and production method therefor, and nickel electrode and alkaline battery |
| CN1226795C (en) * | 2003-06-18 | 2005-11-09 | 南开大学 | Nickel-hydrogen power battery |
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