CN105152231A - Method for preparing lithium battery anode material cobaltous hydroxide - Google Patents
Method for preparing lithium battery anode material cobaltous hydroxide Download PDFInfo
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- CN105152231A CN105152231A CN201510597552.XA CN201510597552A CN105152231A CN 105152231 A CN105152231 A CN 105152231A CN 201510597552 A CN201510597552 A CN 201510597552A CN 105152231 A CN105152231 A CN 105152231A
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- cobalt
- cobaltous hydroxide
- lithium battery
- cobaltous
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- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 title claims abstract description 62
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 title claims abstract description 50
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 19
- 239000010405 anode material Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 59
- 229910017052 cobalt Inorganic materials 0.000 claims description 45
- 239000010941 cobalt Substances 0.000 claims description 45
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 26
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 22
- 239000004202 carbamide Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000012456 homogeneous solution Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- 238000007654 immersion Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 5
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 229910001429 cobalt ion Inorganic materials 0.000 description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 235000011089 carbon dioxide Nutrition 0.000 description 2
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+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 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000011426 transformation method Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- -1 hydroxide radical Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for preparing a lithium battery anode material cobaltous hydroxide. The method comprises the following steps: 1) performing hydrolytic precipitation to prepare a crystal nucleus; 2) performing homogeneous precipitation; 3) performing alkali washing; and 4) performing after-treatment. A cobaltous hydroxide crystal nucleus which is uniform in particle size distribution can be prepared through hydrolytic precipitation, and the cobaltous hydroxide crystal nucleus can be further added into a reaction kettle to prepare large-particle cobaltous hydroxide through homogeneous precipitation. By adopting the method for preparing the lithium battery anode material cobaltous hydroxide, the prepared cobaltous hydroxide is narrow in particle size distribution and good in degree of sphericity.
Description
Technical field
The present invention relates to new energy materials preparation field, be specifically related to the preparation method of anode material of lithium battery cobaltous hydroxide.
Background technology
Cobaltous hydroxide is a kind of presoma of important anode material of lithium battery, for the production of lithium cobaltate cathode lithium battery material.Along with the fast development of China's economic society, the parent that green energy resource is subject to people relies, and battery industry grows continuously and fast, and the Application Areas of cobaltous hydroxide is constantly expanded in addition, and the demand in market is also increasing.
Method prepared by the cobaltous hydroxide of present has the alkali lye precipitator method, precipitation transformation method etc.Patent of invention CN1190947 as H.C. Starck GmbH & Co. KG discloses and adopts precipitation transformation method to prepare Large stone cobaltous hydroxide, first cobalt salt and carbonate or supercarbonate is used to form cobaltous dihydroxycarbonate, after washing drying, cobaltous dihydroxycarbonate is pulled an oar, then mix with NaOH solution, after washing, product needs vacuum dehydrating at lower temperature.This method production process is long, and drying conditions is harsh, is unfavorable for suitability for industrialized production.Therefore prior art Problems existing has: 1. the size-grade distribution of cobaltous hydroxide is too wide; 2. the sphericity of cobaltous hydroxide is bad.
Summary of the invention
For above Problems existing, the object of the present invention is to provide the preparation method of anode material of lithium battery cobaltous hydroxide.Cobaltous hydroxide narrow particle size distribution prepared by present method, flow process is short, and cost is low, the good sphericity of cobaltous hydroxide.
The technical solution used in the present invention is as follows:
The preparation method of anode material of lithium battery cobaltous hydroxide, is characterized in that, comprises following step:
1) hydrolytic precipitation prepares nucleus, adds in pure water, then add dispersion agent by Virahol cobalt, starts to stir simultaneously, and mixing speed is 500-1200r/min, at 30-99 DEG C of reaction 2-10 hour, obtains cobaltous hydroxide precipitation and does nucleus;
2) precipitation from homogeneous solution (PFHS), doubly adding pure water pulp by obtaining the 2-10 of cobaltous hydroxide nucleus according to its quality, then pure cobalt liquor and urea being added, being warming up to 90-100 DEG C according to the speed of 3-5 DEG C/h, and isothermal reaction 2-10 hour, mixing speed 300-800r/min;
3) alkali cleaning, the material filtering that precipitation from homogeneous solution (PFHS) is obtained, sodium hydroxide solution filter material being added 0.5-3mol/l soaks 2-4 hour, soaking temperature 70-80 DEG C, then by the slurries filtration after immersion;
4) aftertreatment, material after alkali cleaning is added pure water, washing is to water outlet pH6-9, specific conductivity < 50us/cm, the temperature of washing water is 60-80 DEG C, the drying materials after washing, dries to moisture < 0.5%, then cross 150-250 mesh sieve, then pack after batch mixing, deironing.
In described step 1, the concentration of Virahol cobalt in water is 0.25-1mol/l, and the concentration of dispersion agent is 0.01-0.1mol/l.
Cobalt in described step 2 in cobaltous hydroxide nucleus, cobalt liquor and the mol ratio of urea are 1:0.5-10:2-40, cobalt liquor is at least one in cobalt sulfate solution, cobalt chloride solution, cobalt nitrate solution, cobalt acetate solution, the concentration of cobalt liquor is 0.5-1mol/l, and the concentration of urea is 1-3mol/l.
In described step 3, in cobaltous hydroxide and sodium hydroxide solution, the mol ratio of sodium hydroxide is 1:0.2-1.
In described step 4, bake out temperature is 60-120 DEG C.
Principle of the present invention is as follows:
Virahol cobalt is the organic salt of cobalt, and it hydrolysis reaction can occur in water, obtains cobaltous hydroxide subparticle, and because this hydrolysis is by parameters such as control temperature, thus the granularity of controlled hydrogen manufacturing cobalt oxide particle obtains nucleus.
Due to urea in aqueous, can slowly resolve into carbonic acid gas and ammonia under the high temperature conditions, carbonic acid gas is difficult to be dissolved in water and the water surface of overflowing, ammonia is dissolved in water because the solubleness in water is comparatively large, thus formation ammonia solution, and ammonia solution can ionize out hydroxide ion, thus make cobalt ion precipitation obtain cobaltous hydroxide, owing to controlling the decomposition of urea soln by control temperature and heat-up rate, thus indirectly control the sedimentation speed of cobalt ion, and be uniformly distributed in urea soln due to urea, cobalt ion is also uniformly distributed in the solution, the hydroxide radical that the ammonia then produced ionizes out is also uniformly distributed in the solution, avoid local over-concentration phenomenon, make the throw out size-grade distribution of cobalt evenly, and be spherical, its chemical equation occurred is as follows:
CO(NH
2)
2+H
2O=CO
2+NH
3
NH3+H2O=NH3.H2O<------>NH
4++OH
-
Co
2++2OH
------->Co(OH)
2
And speed of response can be controlled due to reaction, thus newly-generated cobaltous hydroxide can be controlled grow on nucleus, obtain the cobaltous hydroxide particle of homogeneous grain diameter.
The invention has the beneficial effects as follows: the narrow particle size distribution of cobaltous hydroxide prepared by present method, flow process is short, and cost is low, the good sphericity of cobaltous hydroxide.
Embodiment
embodiment 1
The preparation method of anode material of lithium battery cobaltous hydroxide, is characterized in that, comprises following step:
1) hydrolytic precipitation prepares nucleus, adds in pure water, then add dispersion agent by Virahol cobalt, starts to stir simultaneously, and mixing speed is 700r/min, 80 DEG C of reactions 5 hours, obtains cobaltous hydroxide precipitation and does nucleus;
2) precipitation from homogeneous solution (PFHS), adding pure water pulp by obtaining cobaltous hydroxide nucleus according to 8 times of its quality, then pure cobalt liquor and urea being added, being warming up to 99 DEG C according to the speed of 3.5 DEG C/h, and isothermal reaction 6 hours, mixing speed 700r/min;
3) alkali cleaning, the material filtering that precipitation from homogeneous solution (PFHS) is obtained, sodium hydroxide solution filter material being added 0.9mol/l soaks 3 hours, soaking temperature 75 DEG C, then by the slurries filtration after immersion;
4) aftertreatment, material after alkali cleaning is added pure water, and wash to water outlet pH7.5, specific conductivity 40us/cm, the temperature of washing water is 75 DEG C, the drying materials after washing, dries to moisture 0.3%, then crosses 225 mesh sieve, then packs after batch mixing, deironing.
In described step 1, the concentration of Virahol cobalt in water is 0.5mol/l, and the concentration of dispersion agent is 0.03mol/l.
Cobalt in described step 2 in cobaltous hydroxide nucleus, cobalt liquor and the mol ratio of urea are 1:2.5:10, and cobalt liquor is cobalt sulfate solution, and the concentration of cobalt liquor is 0.8mol/l, and the concentration of urea is 1.3mol/l.
In described step 3, in cobaltous hydroxide and sodium hydroxide solution, the mol ratio of sodium hydroxide is 1:0.8.
In described step 4, bake out temperature is 110 DEG C.
The cobaltous hydroxide index finally obtained is as follows:
| Index | D50 | (D90-D10)/D50 | SO 4 2- | Fe | Na |
| Numerical value | 10.2um | 0.55 | 0.025% | 0.0011% | 0.010% |
Embodiment 2
The preparation method of anode material of lithium battery cobaltous hydroxide, is characterized in that, comprises following step:
1) hydrolytic precipitation prepares nucleus, adds in pure water, then add dispersion agent by Virahol cobalt, starts to stir simultaneously, and mixing speed is 1100r/min, 85 DEG C of reactions 6 hours, obtains cobaltous hydroxide precipitation and does nucleus;
2) precipitation from homogeneous solution (PFHS), adding pure water pulp by obtaining cobaltous hydroxide nucleus according to 5 times of its quality, then pure cobalt liquor and urea being added, being warming up to 97 DEG C according to the speed of 4 DEG C/h, and isothermal reaction 5 hours, mixing speed 500r/min;
3) alkali cleaning, the material filtering that precipitation from homogeneous solution (PFHS) is obtained, sodium hydroxide solution filter material being added 2.5mol/l soaks 3 hours, soaking temperature 78 DEG C, then by the slurries filtration after immersion;
4) aftertreatment, material after alkali cleaning is added pure water, and wash to water outlet pH8.5, specific conductivity 35us/cm, the temperature of washing water is 75 DEG C, the drying materials after washing, dries to moisture 0.3%, then crosses 200 mesh sieve, then packs after batch mixing, deironing.
In described step 1, the concentration of Virahol cobalt in water is 0.85mol/l, and the concentration of dispersion agent is 0.05mol/l.
Cobalt in described step 2 in cobaltous hydroxide nucleus, cobalt liquor and the mol ratio of urea are 1:5:20, and cobalt liquor is Cobaltous diacetate, and the concentration of cobalt liquor is 0.65mol/l, and the concentration of urea is 2.5mol/l.
In described step 3, in cobaltous hydroxide and sodium hydroxide solution, the mol ratio of sodium hydroxide is 1:0.8.
In described step 4, bake out temperature is 75 DEG C.
The cobaltous hydroxide index finally obtained is as follows:
| Index | D50 | (D90-D10)/D50 | SO 4 2- | Fe | Na |
| Numerical value | 12.2um | 0.58 | 0.047% | 0.0011% | 0.0085% |
Embodiment 3
The preparation method of anode material of lithium battery cobaltous hydroxide, is characterized in that, comprises following step:
1) hydrolytic precipitation prepares nucleus, adds in pure water, then add dispersion agent by Virahol cobalt, starts to stir simultaneously, and mixing speed is 900r/min, 65 DEG C of reactions 7 hours, obtains cobaltous hydroxide precipitation and does nucleus;
2) precipitation from homogeneous solution (PFHS), adding pure water pulp by obtaining cobaltous hydroxide nucleus according to 6 times of its quality, then pure cobalt liquor and urea being added, being warming up to 98 DEG C according to the speed of 4 DEG C/h, and isothermal reaction 7 hours, mixing speed 750r/min;
3) alkali cleaning, the material filtering that precipitation from homogeneous solution (PFHS) is obtained, sodium hydroxide solution filter material being added 2mol/l soaks 3.5 hours, soaking temperature 80 DEG C, then by the slurries filtration after immersion;
4) aftertreatment, material after alkali cleaning is added pure water, and wash to water outlet pH8.5, specific conductivity 35us/cm, the temperature of washing water is 73 DEG C, the drying materials after washing, dries to moisture 0.45%, then crosses 150 mesh sieve, then packs after batch mixing, deironing.
In described step 1, the concentration of Virahol cobalt in water is 0.85mol/l, and the concentration of dispersion agent is 0.08mol/l.
Cobalt in described step 2 in cobaltous hydroxide nucleus, cobalt liquor and the mol ratio of urea are 1:7:30, and cobalt liquor is cobalt acetate solution, and the concentration of cobalt liquor is 0.85mol/l, and the concentration of urea is 1.9mol/l.
In described step 3, in cobaltous hydroxide and sodium hydroxide solution, the mol ratio of sodium hydroxide is 1:0.8.
In described step 4, bake out temperature is 70 DEG C.
The cobaltous hydroxide index finally obtained is as follows:
| Index | D50 | (D90-D10)/D50 | SO 4 2- | Fe | Na |
| Numerical value | 14.5um | 0.67 | 0.023% | 0.0012% | 0.0097% |
Embodiment 4
The preparation method of anode material of lithium battery cobaltous hydroxide, is characterized in that, comprises following step:
1) hydrolytic precipitation prepares nucleus, adds in pure water, then add dispersion agent by Virahol cobalt, starts to stir simultaneously, and mixing speed is 800r/min, 65 DEG C of reactions 6 hours, obtains cobaltous hydroxide precipitation and does nucleus;
2) precipitation from homogeneous solution (PFHS), adding pure water pulp by obtaining cobaltous hydroxide nucleus according to 6 times of its quality, then pure cobalt liquor and urea being added, being warming up to 92 DEG C according to the speed of 4 DEG C/h, and isothermal reaction 7 hours, mixing speed 850r/min;
3) alkali cleaning, the material filtering that precipitation from homogeneous solution (PFHS) is obtained, sodium hydroxide solution filter material being added 2mol/l soaks 3.5 hours, soaking temperature 80 DEG C, then by the slurries filtration after immersion;
4) aftertreatment, material after alkali cleaning is added pure water, and wash to water outlet pH8.5, specific conductivity 35us/cm, the temperature of washing water is 70 DEG C, the drying materials after washing, dries to moisture 0.45%, then crosses 150 mesh sieve, then packs after batch mixing, deironing.
In described step 1, the concentration of Virahol cobalt in water is 0.85mol/l, and the concentration of dispersion agent is 0.08mol/l.
Cobalt in described step 2 in cobaltous hydroxide nucleus, cobalt liquor and the mol ratio of urea are 1:6:30, and cobalt liquor is cobalt acetate solution, and the concentration of cobalt liquor is 0.75mol/l, and the concentration of urea is 1.9mol/l.
In described step 3, in cobaltous hydroxide and sodium hydroxide solution, the mol ratio of sodium hydroxide is 1:0.8.
In described step 4, bake out temperature is 80 DEG C.
The cobaltous hydroxide index finally obtained is as follows:
| Index | D50 | (D90-D10)/D50 | SO 4 2- | Fe | Na |
| Numerical value | 13.2um | 0.62 | 0.029% | 0.0015% | 0.0091% |
Claims (5)
1. the preparation method of anode material of lithium battery cobaltous hydroxide, is characterized in that, comprises following step:
1) hydrolytic precipitation prepares nucleus, adds in pure water, then add dispersion agent by Virahol cobalt, starts to stir simultaneously, and mixing speed is 500-1200r/min, at 30-99 DEG C of reaction 2-10 hour, obtains cobaltous hydroxide precipitation and does nucleus;
2) precipitation from homogeneous solution (PFHS), doubly adding pure water pulp by obtaining the 2-10 of cobaltous hydroxide nucleus according to its quality, then pure cobalt liquor and urea being added, being warming up to 90-100 DEG C according to the speed of 3-5 DEG C/h, and isothermal reaction 2-10 hour, mixing speed 300-800r/min;
3) alkali cleaning, the material filtering that precipitation from homogeneous solution (PFHS) is obtained, sodium hydroxide solution filter material being added 0.5-3mol/l soaks 2-4 hour, soaking temperature 70-80 DEG C, then by the slurries filtration after immersion;
4) aftertreatment, material after alkali cleaning is added pure water, washing is to water outlet pH6-9, specific conductivity < 50us/cm, the temperature of washing water is 60-80 DEG C, the drying materials after washing, dries to moisture < 0.5%, then cross 150-250 mesh sieve, then pack after batch mixing, deironing.
2. the preparation method of anode material of lithium battery cobaltous hydroxide according to claim 1, is characterized in that, in described step 1, the concentration of Virahol cobalt in water is 0.25-1mol/l, and the concentration of dispersion agent is 0.01-0.1mol/l.
3. the preparation method of anode material of lithium battery cobaltous hydroxide according to claim 1, it is characterized in that, cobalt in described step 2 in cobaltous hydroxide nucleus, cobalt liquor and the mol ratio of urea are 1:0.5-10:2-40, cobalt liquor is at least one in cobalt sulfate solution, cobalt chloride solution, cobalt nitrate solution, cobalt acetate solution, the concentration of cobalt liquor is 0.5-1mol/l, and the concentration of urea is 1-3mol/l.
4. the preparation method of anode material of lithium battery cobaltous hydroxide according to claim 1, is characterized in that, in described step 3, in cobaltous hydroxide and sodium hydroxide solution, the mol ratio of sodium hydroxide is 1:0.2-1.
5. the preparation method of anode material of lithium battery cobaltous hydroxide according to claim 1, is characterized in that, in described step 4, bake out temperature is 60-120 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395754A (en) * | 2016-11-16 | 2017-02-15 | 天津巴莫科技股份有限公司 | Preparation method of mono-/multi-metal coprecipitation hydroxide or carbonate |
| CN107871860A (en) * | 2017-11-02 | 2018-04-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method using metatitanic acid lithium cladding manganese cobalt oxide and products thereof and application |
| CN109686966A (en) * | 2018-12-05 | 2019-04-26 | 华友新能源科技（衢州）有限公司 | A kind of energy storage super large partial size nickel cobalt manganese hydroxide and preparation method thereof |
| CN111446438A (en) * | 2020-04-30 | 2020-07-24 | 青海民族大学 | Lithium battery positive electrode material and preparation method thereof |
| CN114335482A (en) * | 2021-12-28 | 2022-04-12 | 陕西科技大学 | MnO (MnO)2-metal heterojunction composite material and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190947A (en) * | 1995-05-26 | 1998-08-19 | H·C·施塔克公司 | Spheroidally agglomerated basic cobalt (II) carbonate and spheroidally agglomerated cobalt (II) hydroxide, process for their production and their use |
| CN101746787A (en) * | 2008-12-08 | 2010-06-23 | 广州慧谷化学有限公司 | Preparation method of nanometer aluminium hydroxide and application thereof |
| CN101921001A (en) * | 2010-09-17 | 2010-12-22 | 浙江华友钴业股份有限公司 | Technology for preparing cobalt hydroxide from cobaltous sulfate solution |
| CN104445442A (en) * | 2014-12-09 | 2015-03-25 | 英德佳纳金属科技有限公司 | Cobalt hydroxide with low chlorine/sulfur and large particle size and preparation method thereof |
-
2015
- 2015-09-20 CN CN201510597552.XA patent/CN105152231B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190947A (en) * | 1995-05-26 | 1998-08-19 | H·C·施塔克公司 | Spheroidally agglomerated basic cobalt (II) carbonate and spheroidally agglomerated cobalt (II) hydroxide, process for their production and their use |
| CN101746787A (en) * | 2008-12-08 | 2010-06-23 | 广州慧谷化学有限公司 | Preparation method of nanometer aluminium hydroxide and application thereof |
| CN101921001A (en) * | 2010-09-17 | 2010-12-22 | 浙江华友钴业股份有限公司 | Technology for preparing cobalt hydroxide from cobaltous sulfate solution |
| CN104445442A (en) * | 2014-12-09 | 2015-03-25 | 英德佳纳金属科技有限公司 | Cobalt hydroxide with low chlorine/sulfur and large particle size and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| MRIDULA DIXIT ET AL.: ""Homogeneous precipitation from solution by urea hydrolysis: a novel chemical route to the a-hydroxides of nickel and cobalt"", 《J. MUTER. CHEM.》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395754A (en) * | 2016-11-16 | 2017-02-15 | 天津巴莫科技股份有限公司 | Preparation method of mono-/multi-metal coprecipitation hydroxide or carbonate |
| CN106395754B (en) * | 2016-11-16 | 2018-11-20 | 天津巴莫科技股份有限公司 | Mono-/multi- metal is co-precipitated the preparation method of hydroxide or carbonated |
| CN107871860A (en) * | 2017-11-02 | 2018-04-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method using metatitanic acid lithium cladding manganese cobalt oxide and products thereof and application |
| CN109686966A (en) * | 2018-12-05 | 2019-04-26 | 华友新能源科技（衢州）有限公司 | A kind of energy storage super large partial size nickel cobalt manganese hydroxide and preparation method thereof |
| CN111446438A (en) * | 2020-04-30 | 2020-07-24 | 青海民族大学 | Lithium battery positive electrode material and preparation method thereof |
| CN111446438B (en) * | 2020-04-30 | 2021-08-03 | 青海民族大学 | Lithium battery positive electrode material and preparation method thereof |
| CN114335482A (en) * | 2021-12-28 | 2022-04-12 | 陕西科技大学 | MnO (MnO)2-metal heterojunction composite material and preparation method and application thereof |
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