CN103165878A - Preparation method of spherical nickel-manganese binary material - Google Patents
Preparation method of spherical nickel-manganese binary material Download PDFInfo
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- CN103165878A CN103165878A CN2013100966915A CN201310096691A CN103165878A CN 103165878 A CN103165878 A CN 103165878A CN 2013100966915 A CN2013100966915 A CN 2013100966915A CN 201310096691 A CN201310096691 A CN 201310096691A CN 103165878 A CN103165878 A CN 103165878A
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Abstract
The invention relates to the field of lithium ion battery materials and particularly relates to a preparation method of a spherical nickel-manganese binary material. The preparation method comprises the following steps: continuously pumping a sodium hydroxide solution, a complexing agent solution and a mixed water solution of a nickel salt and a manganese salt into a bottom liquid together in a parallel-flow manner, performing precipitation reaction, controlling the stirring rational speed, the alkali degree and the pH value of a reaction system and the like, enabling reactants to produce a crystal nucleus, enabling the crystal nucleus to grow into spherical particles, enabling a reaction material solution to continuously flow out and enter an aging kettle from the overflow port at the upper part of a reaction kettle, washing and drying to get a spherical nickel-manganese hydroxide; and uniformly mixing the spherical nickel-manganese hydroxide with a lithium source, performing high-temperature calcination under oxygen-introducing conditions, and grinding after calcination to get the spherical nickel-manganese binary material. The spherical nickel-manganese binary material has the advantages of high voltage, better sphericity, high tap density, long cycle life and good safety performance. In addition, the preparation method has the advantages of low requirements on synthesis equipment, simple process flow, easiness in control of reaction, high production efficiency and simpler sintering process, is suitable for continuous industrial production and has very broad development prospects and larger market potential.
Description
Technical field
The present invention relates to the lithium ion battery material field, particularly a kind of preparation method of spherical nickel manganese binary material.
Background technology
Since layer structure cobalt acid lithium was made battery that positive electrode makes and put goods on the market, lithium ion battery demonstrated importance day by day in every field, and battery material is fast-developing, the lithium ion battery material of various characteristics in succession occurs.As LiMn2O4, lithium nickelate, lithium nickel cobalt dioxide, LiFePO 4, nickel-cobalt-manganese ternary material etc.People are also more and more higher to the requirement of lithium ion battery, and people need to use the lithium ion battery that price is low, size is less, cycle life is longer, weight is lighter.And present existing lithium ion battery material can't satisfy above performance simultaneously, only has lithium nickelate can satisfy above most requirement.Because the price of nickel is relatively high, can't satisfy people's requirement low to price.Therefore in the present invention, manganese has been replaced the nickel of part, the spherical nickel manganese binary material of preparing has not only possessed the outstanding properties that lithium nickelate has, and has improved the safety and stability of positive electrode due to adding of manganese, the cost that has also reduced.
Summary of the invention
In order to solve the technical problem that exists in prior art, the object of the present invention is to provide a kind of technological process simple, reaction is easy to control, sphericity is better, and tap density is high, have extended cycle life, the preparation method of the good and spherical nickel manganese binary material that suitable continuous industrial is produced of security performance.
The technical solution used in the present invention is as follows:
A kind of preparation method of spherical nickel manganese binary material is characterized in that, comprises the steps:
1., take pure water as end liquid, Temperature Setting is 40～80 ℃, controlling speed of agitator is 100～250 r/min, adds enveloping agent solution and sodium hydroxide solution to regulate end liquid caustic soda degree to 25～45 g/l, the pH value is 10.5～12.0;
2., nickel salt and manganese salt are dissolved into mixed aqueous solution, mix rear total concentration of metal ions and be controlled to be 0.5～2.0 mol/l, again with sodium hydroxide solution, enveloping agent solution and mixed aqueous solution continuous and stream together pump in end liquid, 40～80 ℃ precipitation reaction occurs, controlling speed of agitator is 100～250 r/min, control the basicity of reaction system, pH value and solids in pulp amount, make reactant produce nucleus, nucleus growth is spheric granules, the reaction feed liquid enters aging reactor by continuous outflow of reactor top overfall, dry through washing press washing and vacuum drier, obtain spherical nickel manganese hydroxide,
3., with spherical nickel manganese hydroxide and lithium source mixing, high-temperature calcination under logical oxygen condition, calcining obtains spherical nickel manganese binary material after grinding.
Preferably, described nickel salt is nickelous sulfate, nickel chloride or nickel nitrate; Described manganese salt is manganese sulfate, manganese chloride or manganese nitrate.
Further, the mol ratio of described nickel salt, manganese salt is 60～90:10～40.
Preferably, described enveloping agent solution is that concentration is 5～25% ammoniacal liquor or ammonium salt solution.
Preferably, the concentration of described sodium hydroxide solution is 10～30%.
Further, controlling pH value of reaction system is 10.5～12.0, and basicity is 25～45 g/l, and the solids in pulp amount is 100～300 g/l.
Further, the hot deionized water pH value of reaction feed liquid after washing press press filtration washing is controlled to be 7.5～8.5, and the vacuum drier temperature is controlled to be 90～110 ℃.
Further, the mol ratio in spherical nickel manganese hydroxide and lithium source is 1.02～1.08:1, and the lithium source is one or more in battery-level lithium carbonate, lithium hydroxide or lithium nitrate.
Further, under logical oxygen condition, the temperature of high-temperature calcination is controlled to be 750～950 ℃, and calcination time is 12～25 h.
Comparatively perfect is that the tap density of described spherical nickel manganese binary material is 2.0～2.8 g/cm
3, granularity is 5～25 μ m.
The spherical nickel manganese binary material of the present invention preparation has voltage high, and sphericity is better, and tap density is high, has extended cycle life, and security performance is good.In addition, the present invention is low to the synthesis device requirement, technological process is simple, and reaction is easy to control, and production efficiency is high, and sintering process is simpler, is fit to continuous industrial production, has very vast potential for future development, and market potential is larger.
Description of drawings
For the ease of it will be appreciated by those skilled in the art that the present invention is further illustrated below in conjunction with accompanying drawing.
Fig. 1 is the Electronic Speculum figure of the embodiment of the present invention 1 preparing product.
Embodiment
Embodiment 1
1., take pure water as end liquid, Temperature Setting is 60 ℃, controlling speed of agitator is 145～155 r/min, add 10% ammoniacal liquor (volumn concentration, lower with) and concentration be the 20%(weight percentage, sodium hydroxide solution down together) is regulated end liquid caustic soda degree to 30 g/l, and the pH value is 10.5～11.0.
2., with nickelous sulfate and manganese chloride in molar ratio for 4:1 is dissolved into mixed aqueous solution, mix rear total concentration of metal ions and be controlled to be 1 mol/l.
With concentration be again 20% sodium hydroxide solution, 10% ammoniacal liquor and mixed aqueous solution together continuously and stream pump in end liquid, 60 ℃ precipitation reaction occurs, controlling speed of agitator is 145～155 r/min, the basicity of controlling reaction system is that 28～32 g/l, pH value are 10.5～11.0, and the solids in pulp amount is 140～160 g/l.
Make reactant produce nucleus, nucleus growth is spheric granules, and the reaction feed liquid enters aging reactor by continuous outflow of reactor top overfall, and is dry through washing press washing and vacuum drier, thereby obtains spherical nickel manganese hydroxide.Hot deionized water pH value after the press filtration washing is controlled to be 7.5～8.0, and the vacuum drier temperature is controlled to be 90～100 ℃.
3., be the 1.02:1 mixing in molar ratio with spherical nickel manganese hydroxide and lithium nitrate, high-temperature calcination under logical oxygen condition, the temperature of high-temperature calcination is controlled to be 740～760 ℃, calcination time is 12 h, and calcining is 2.0～2.2 g/cm by the tap density of the spherical nickel manganese binary material that obtains after grinding
3, granularity is 5～15 μ m.
See also Fig. 1, this spherical nickel manganese binary material, good sphericity, tap density is high.
Embodiment 2
1., take pure water as end liquid, Temperature Setting is 70 ℃, and controlling speed of agitator is 195～205 r/min, adds 15% ammonium salt solution (weight percentage, lower with) and concentration be 25% sodium hydroxide solution adjusting end liquid caustic soda degree to 35 g/l, the pH value is 11.0～11.5.
2., with nickel nitrate and manganese sulfate in molar ratio for 7:3 is dissolved into mixed aqueous solution, mix rear total concentration of metal ions and be controlled to be 1.5 mol/l.
With concentration be again 25% sodium hydroxide solution, 15% ammonium salt solution and mixed aqueous solution together continuously and stream pump in end liquid, 70 ℃ precipitation reaction occurs, controlling speed of agitator is 195～205 r/min, the basicity of controlling reaction system is that 33～37 g/l, pH value are 11.0～11.5, and the solids in pulp amount is 190～210 g/l.
Make reactant produce nucleus, nucleus growth is spheric granules, and the reaction feed liquid enters aging reactor by continuous outflow of reactor top overfall, and is dry through washing press washing and vacuum drier, thereby obtains spherical nickel manganese hydroxide.Hot deionized water pH value after the press filtration washing is controlled to be 7.5～8.5, and the vacuum drier temperature is controlled to be 95～105 ℃.
3., be the 1.07:1 mixing in molar ratio with spherical nickel manganese hydroxide and lithium hydroxide, high-temperature calcination under logical oxygen condition, the temperature of high-temperature calcination is controlled to be 840～860 ℃, calcination time is 18 h, and calcining is 2.3～2.5 g/cm by the tap density of the spherical nickel manganese binary material that obtains after grinding
3, granularity is 8～16 μ m.
Embodiment 3
1., take pure water as end liquid, Temperature Setting is 75 ℃, controlling speed of agitator is 235～245 r/min, adding 15% ammonium salt solution and concentration is that 25% sodium hydroxide solution is regulated end liquid caustic soda degree to 40 g/l, the pH value is 11.2～11.7.
2., with nickel nitrate and manganese chloride in molar ratio for 3:2 is dissolved into mixed aqueous solution, mix rear total concentration of metal ions and be controlled to be 1.5 mol/l.
With concentration be again 25% sodium hydroxide solution, 15% ammonium salt solution and mixed aqueous solution together continuously and stream pump in end liquid, 75 ℃ precipitation reaction occurs, controlling speed of agitator is 235～245 r/min, the basicity of controlling reaction system is that 38～42 g/l, pH value are 11.2～11.7, and the solids in pulp amount is 235～245 g/l.
Make reactant produce nucleus, nucleus growth is spheric granules, and the reaction feed liquid enters aging reactor by continuous outflow of reactor top overfall, and is dry through washing press washing and vacuum drier, thereby obtains spherical nickel manganese hydroxide.Hot deionized water pH value after the press filtration washing is controlled to be 8.0～9.0, and the vacuum drier temperature is controlled to be 100～110 ℃.
3., be the 1.05:1 mixing in molar ratio with spherical nickel manganese hydroxide and battery-level lithium carbonate, high-temperature calcination under logical oxygen condition, the temperature of high-temperature calcination is controlled to be 890～910 ℃, calcination time is 20 h, and calcining is 2.4～2.7 g/cm by the tap density of the spherical nickel manganese binary material that obtains after grinding
3, granularity is 10～25 μ m.
Above content is only that the present invention is conceived example and explanation; affiliated those skilled in the art make various modifications to described specific embodiment or replenish or adopt similar mode to substitute; only otherwise depart from the design of invention or surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Claims (10)
1. the preparation method of a spherical nickel manganese binary material, is characterized in that, comprises the steps:
1., take pure water as end liquid, Temperature Setting is 40～80 ℃, controlling speed of agitator is 100～250 r/min, adds enveloping agent solution and sodium hydroxide solution to regulate end liquid caustic soda degree to 25～45 g/l, the pH value is 10.5～12.0;
2., nickel salt and manganese salt are dissolved into mixed aqueous solution, mix rear total concentration of metal ions and be controlled to be 0.5～2.0 mol/l, again with sodium hydroxide solution, enveloping agent solution and mixed aqueous solution continuous and stream together pump in end liquid, 40～80 ℃ precipitation reaction occurs, controlling speed of agitator is 100～250 r/min, control the basicity of reaction system, pH value and solids in pulp amount, make reactant produce nucleus, nucleus growth is spheric granules, the reaction feed liquid enters aging reactor by continuous outflow of reactor top overfall, dry through washing press washing and vacuum drier, obtain spherical nickel manganese hydroxide,
3., with spherical nickel manganese hydroxide and lithium source mixing, high-temperature calcination under logical oxygen condition, calcining obtains spherical nickel manganese binary material after grinding.
2. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, is characterized in that, described nickel salt is nickelous sulfate, nickel chloride or nickel nitrate; Described manganese salt is manganese sulfate, manganese chloride or manganese nitrate.
3. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, is characterized in that, the mol ratio of described nickel salt, manganese salt is 60～90:10～40.
4. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, is characterized in that, described enveloping agent solution is that concentration is 5～25% ammoniacal liquor or ammonium salt solution.
5. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, is characterized in that, the concentration of described sodium hydroxide solution is 10～30%.
6. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, is characterized in that, controlling pH value of reaction system is 10.5～12.0, and basicity is 25～45 g/l, and the solids in pulp amount is 100～300 g/l.
7. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, is characterized in that, the hot deionized water pH value of reaction feed liquid after washing press press filtration washing is controlled to be 7.5～8.5, and the vacuum drier temperature is controlled to be 90～110 ℃.
8. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, it is characterized in that, the mol ratio in spherical nickel manganese hydroxide and lithium source is 1.02～1.08:1, and the lithium source is one or more in battery-level lithium carbonate, lithium hydroxide or lithium nitrate.
9. the preparation method of a kind of spherical nickel manganese binary material according to claim 1, is characterized in that, under logical oxygen condition, the temperature of high-temperature calcination is controlled to be 750～950 ℃, and calcination time is 12～25 h.
10. the preparation method of the described a kind of spherical nickel manganese binary material of according to claim 1～9 any one, is characterized in that, the tap density of described spherical nickel manganese binary material is 2.0～2.8 g/cm
3, granularity is 5～25 μ m.
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| CN103456946A (en) * | 2013-09-12 | 2013-12-18 | 刘志航 | Anode material for lithium ion battery |
| CN104779388A (en) * | 2015-04-30 | 2015-07-15 | 湖南瑞翔新材料股份有限公司 | Nickel and cobalt binary anode material precursor preparing method and nickel and cobalt binary anode material precursor prepared through method |
| CN105118981A (en) * | 2015-04-30 | 2015-12-02 | 宁夏东方钽业股份有限公司 | High-capacity nickel-cobalt-lithium manganate precursor and preparation method thereof |
| CN107256965A (en) * | 2017-06-22 | 2017-10-17 | 芜湖浙鑫新能源有限公司 | A kind of high pure spherical nickel ion doped prepared based on annealing method and preparation method thereof |
| CN107973349A (en) * | 2017-11-24 | 2018-05-01 | 贵州大龙汇成新材料有限公司 | A kind of nickel manganese binary presoma for mixing aluminium and preparation method thereof |
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| CN109311696A (en) * | 2016-07-20 | 2019-02-05 | 托普索公司 | The scalable depositing synthesis process of battery material with adjustable particle size distribution |
| CN109970107A (en) * | 2019-04-04 | 2019-07-05 | 中科(马鞍山)新材科创园有限公司 | A kind of lithium-rich manganese-based anode material, and its preparation method and application |
| CN112299494A (en) * | 2020-10-29 | 2021-02-02 | 格林爱科(荆门)新能源材料有限公司 | Preparation method of nickel-cobalt hydroxide material |
| CN112537805A (en) * | 2020-12-22 | 2021-03-23 | 浙江帕瓦新能源股份有限公司 | Preparation method of modified nickel-manganese binary precursor |
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| CN115959716A (en) * | 2022-12-06 | 2023-04-14 | 中钢天源股份有限公司 | Nickel-manganese binary precursor and preparation method thereof |
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| CN115725866A (en) * | 2022-11-21 | 2023-03-03 | 北京工业大学 | Method for preferentially recovering manganese from waste lithium-rich manganese-based positive electrode material |
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