CN102810674A - Preparation method of Al-coated nickel-cobalt binary material - Google Patents
Preparation method of Al-coated nickel-cobalt binary material Download PDFInfo
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Abstract
The invention relates to the field of a lithium ion battery material, in particular to a preparation method of an Al-coated nickel-cobalt binary material. Al is coated by adopting a wet method, pure water is adopted as base solution, a nickel-cobalt binary material is used as a base material, the temperature is controlled at 40-80 DEG C, the mixing speed is controlled as 80-160r/min, ammonia is added to adjust the alkalinity of the base solution to be 20-40g/L, the pH (Potential of Hydrogen) is controlled to be 10.50-11.5, aluminum sulfate solution with the concentration of 60-100g/L, sodium hydroxide solution of 15-30 percent and ammonia of 10-25 percent are continuously pumped together into the base solution, aluminum hydroxide precipitation reaction is performed at 40-80 DEG C, aluminum hydroxide deposits are grown on the surface of the nickel-cobalt binary material, and the Al2O3-coated nickel-cobalt binary material is obtained by washing, pressure filtration, drying and re-calcination of the prepared solution. The process flow is relatively simple, and the reaction can be controlled easily. Compared with the existing Al coating through a dry method, Al can be distributed more uniformly in the nickel-cobalt binary material, the product consistency is better, the tap density is higher, and the electrical performance is excellent and more stable.
Description
Technical field
The present invention relates to the lithium ion battery material field, particularly a kind of preparation method who wraps the nickel cobalt binary material of Al.
Background technology
Nickel cobalt binary material is to use comparatively general a kind of material in the anode material for lithium-ion batteries, and prior art is mainly passed through dry coated aluminium oxide processing technology, the nickel cobalt binary material of the bag Al of this prepared, and not only technology is comparatively loaded down with trivial details, simultaneously Al in the product
2O
3Skewness, the product cycle performance is relatively poor and unstable, and tap density is lower.
Summary of the invention
In order to solve the technical problem that exists in the prior art, the object of the present invention is to provide the preparation method of the nickel cobalt binary material of a kind of Al of bag.
The technical scheme that the present invention adopts is following:
A kind of preparation method who wraps the nickel cobalt binary material of Al is characterized in that, comprises the steps:
With the pure water is end liquid, and temperature rises to 40～80 ℃;
The control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 25～45g/L at 80～180r/min, and pH is 11.50～12.50 in control;
Nickel salt and cobalt salt mixed solution, sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid; Precipitation reaction takes place at 40～80 ℃; Slip solid content, basicity and the pH of control reaction system; The reaction feed liquid flows out the entering aging reactor continuously by agitated reactor top overfall, and is dry through washing press washing and vacuum drier, obtains spherical nickel-cobalt hydroxide;
Spherical nickel-cobalt hydroxide obtains nickel cobalt binary material through joining the lithium calcining;
Adopting wet method to coat Al, is end liquid with the pure water, and nickel cobalt binary material is a base-material; Temperature is controlled at 40～80 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 20～40g/L at 80～160r/min; PH is 10.50～11.50 in control, aluminum sulfate solution, sodium hydroxide solution and ammoniacal liquor is also flowed continuously pump in the end liquid, the aluminum hydroxide precipitation reaction takes place and be grown in nickel cobalt binary material surface at 40～80 ℃; The gained feed liquid is calcining once more after the washing and filter pressing oven dry, can obtain being coated with Al
2O
3Nickel cobalt binary material.
Preferably, described nickel salt is nickelous sulfate, nickel chloride or nickel nitrate; Cobalt salt is cobaltous sulfate, cobalt chloride or cobalt nitrate.
Further, the mixed solution concentration of metal ions of described nickel salt and cobalt salt is 60～120g/L, and nickel, cobalt concentration of metal ions ratio are 2～8: 1; The concentration of described sodium hydroxide solution is 15～30%, and the concentration of ammoniacal liquor is 10～25%; The concentration of described aluminum sulfate solution is 60～100g/L.
Further, in the described nickel cobalt hydroxide reaction system, basicity is controlled at 25～45g/L, and the slurry solid content is controlled at 150～300g/L, and pH is 11.50～12.50 in control.
Further, the washing of described spherical nickel-cobalt hydroxide adopt 50～80 ℃ hot deionized water wash to pH 7.50～9.50; Said baking temperature is 80～120 ℃.
Further, described lithium source is a battery-level lithium carbonate, and proportioning is a lithium carbonate: nickel cobalt hydroxide=1～1.08: 1.
Further, the lithium calcining heat of joining of described spherical nickel-cobalt hydroxide is controlled at 400～900 ℃.
Further, the calcining heat behind the described bag Al is controlled at 500～900 ℃.
Further, the tap density of the nickel cobalt binary material of the bag Al of preparation is 2.8～3.5g/cm
3, granularity is 5～20um.
Technological process of the present invention is simpler, and reaction is easy to control, compares with existing dry coated Al, and Al is more evenly distributed in nickel cobalt binary material, and consistency of product is better, and tap density is higher, and electrical property is excellent and more stable.
Description of drawings
For the ease of it will be appreciated by those skilled in the art that the present invention is further described below in conjunction with accompanying drawing.
Fig. 1 is the sem photograph of spherical nickel-cobalt hydroxide.
Fig. 2 is the sem photograph that spherical nickel-cobalt hydroxide is directly joined lithium calcining gained sample.
Fig. 3 is the sem photograph of the nickel cobalt binary material behind the bag Al.
Embodiment
Embodiment 1
With the pure water is end liquid, and temperature rises to 40～60 ℃.
The control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 25～30g/L at 140～165r/min, and pH is 11.80～12.30 in control.
Nickelous sulfate and cobaltous sulfate mixed solution, sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid; Nickelous sulfate and cobaltous sulfate mixed solution concentration of metal ions are 90g/L; Nickel, cobalt concentration of metal ions are than (mol ratio; Be 2: 1 down together), the concentration of sodium hydroxide solution is 30%, and ammonia concn is 10%.
Precipitation reaction takes place at 40～60 ℃; Control reaction system the slip solid content 150～200g/L, control basicity at 25～30g/L; PH is 11.80～12.00 in control; The reaction feed liquid flows out the entering aging reactor continuously by agitated reactor top overfall, in washing press, adopt 50～60 ℃ hot deionized water wash to pH 7.50～8.00.Carry out the vacuum drier drying then, baking temperature is 80～100 ℃, obtains spherical nickel-cobalt hydroxide.See also Fig. 1, the mobility of particle of spherical nickel-cobalt hydroxide is better.
Spherical nickel-cobalt hydroxide is through joining the lithium calcining, and the lithium source is a battery-level lithium carbonate, and proportioning is a lithium carbonate: nickel cobalt hydroxide=1.07: 1, temperature are controlled at 400～600 ℃, and then obtain nickel cobalt binary material.See also Fig. 2, the tap density of nickel cobalt binary material is higher.
Adopting wet method to coat Al, is end liquid with the pure water, and nickel cobalt binary material is a base-material; Temperature is controlled at 60～75 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 26～35g/L at 140～160r/min; PH is 10.50～11.00 in control; With concentration is 90g/L aluminum sulfate solution and 15% sodium hydroxide solution, 22% ammoniacal liquor continuously and stream pump in the end liquid, the aluminum hydroxide precipitations reaction takes place and is grown in nickel cobalt binary material surface at 40～50 ℃, the gained feed liquid is after the washing and filter pressing oven dry; In 500～600 ℃ of calcinings once more, can obtain being coated with Al
2O
3Nickel cobalt binary material.
The tap density of the nickel cobalt binary material of the bag Al of preparation is 2.8～3.5g/cm
3, granularity is 5～20um.Simultaneously, see also Fig. 3, Al
2O
3Distribution uniform in nickel cobalt binary material.
Embodiment 2
With the pure water is end liquid, and temperature rises to 50～70 ℃.
The control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 30～35g/L at 140～180r/min, and pH is 11.50～11.90 in control.
Nickel chloride and cobalt nitrate mixed solution, sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid; Nickel chloride and cobalt nitrate mixed solution concentration of metal ions are 60g/L; Nickel, cobalt concentration of metal ions ratio are 8: 1, and the concentration of sodium hydroxide solution is 15%, and ammonia concn is 25%.
Precipitation reaction takes place at 50～70 ℃; Control reaction system the slip solid content 180～230g/L, control basicity at 30～35g/L; PH is 11.50～11.75 in control; The reaction feed liquid flows out the entering aging reactor continuously by agitated reactor top overfall, in washing press, adopt 60～70 ℃ hot deionized water wash to pH 9.00～9.50.Carry out the vacuum drier drying then, baking temperature is 90～110 ℃, obtains spherical nickel-cobalt hydroxide.
Spherical nickel-cobalt hydroxide is through joining the lithium calcining, and the lithium source is a battery-level lithium carbonate, and proportioning is a lithium carbonate: nickel cobalt hydroxide=1.05: 1, temperature are controlled at 500～700 ℃, and then obtain nickel cobalt binary material.
Adopting wet method to coat Al, is end liquid with the pure water, and nickel cobalt binary material is a base-material; Temperature is controlled at 50～60 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 35～40g/L at 120～140r/min; PH is 11.00～11.50 in control; With concentration is 100g/L aluminum sulfate solution and 27% sodium hydroxide solution, 12% ammoniacal liquor continuously and stream pump in the end liquid, the aluminum hydroxide precipitations reaction takes place and is grown in nickel cobalt binary material surface at 50～80 ℃, the gained feed liquid is after the washing and filter pressing oven dry; In 500～700 ℃ of calcinings once more, can obtain being coated with Al
2O
3Nickel cobalt binary material.
The tap density of the nickel cobalt binary material of the bag Al of preparation is 2.8～3.5g/cm
3, granularity is 5～20um.
Embodiment 3
With the pure water is end liquid, and temperature rises to 60～80 ℃.
The control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 35～40g/L at 120～160r/min, and pH is 12.10～12.50 in control.
Nickel nitrate and cobaltous sulfate mixed solution, sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid; Nickel nitrate and cobaltous sulfate mixed solution concentration of metal ions are 80g/L; Nickel, cobalt concentration of metal ions ratio are 4: 1, and the concentration of sodium hydroxide solution is 18%, and ammonia concn is 15%.
Precipitation reaction takes place at 60～80 ℃; Control reaction system the slip solid content 200～250g/L, control basicity at 35～40g/L; PH is 11.75～12.05 in control; The reaction feed liquid flows out the entering aging reactor continuously by agitated reactor top overfall, in washing press, adopt 70～80 ℃ hot deionized water wash to pH 8.50～9.00.Carry out the vacuum drier drying then, baking temperature is 100～120 ℃, obtains spherical nickel-cobalt hydroxide.
Spherical nickel-cobalt hydroxide is through joining the lithium calcining, and the lithium source is a battery-level lithium carbonate, and proportioning is a lithium carbonate: nickel cobalt hydroxide=1.03: 1, temperature are controlled at 600～800 ℃, and then obtain nickel cobalt binary material.
Adopting wet method to coat Al, is end liquid with the pure water, and nickel cobalt binary material is a base-material; Temperature is controlled at 65～80 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 30～35g/L at 100～120r/min; PH is 10.50～10.90 in control; With concentration is 80g/L aluminum sulfate solution and 30% sodium hydroxide solution, 25% ammoniacal liquor continuously and stream pump in the end liquid, the aluminum hydroxide precipitations reaction takes place and is grown in nickel cobalt binary material surface at 60～80 ℃, the gained feed liquid is after the washing and filter pressing oven dry; In 600～800 ℃ of calcinings once more, can obtain being coated with Al
2O
3Nickel cobalt binary material.
The tap density of the nickel cobalt binary material of the bag Al of preparation is 2.8～3.5g/cm
3, granularity is 5～20um.
Embodiment 4
With the pure water is end liquid, and temperature rises to 45～65 ℃.
The control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 40～45g/L at 120～140r/min, and pH is 11.70～12.10 in control.
Nickel nitrate and cobalt nitrate mixed solution, sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid; Nickel nitrate and cobalt nitrate mixed solution concentration of metal ions are 100g/L; Nickel, cobalt concentration of metal ions ratio are 5: 1, and the concentration of sodium hydroxide solution is 25%, and ammonia concn is 20%.
Precipitation reaction takes place at 45～65 ℃; Control reaction system the slip solid content 210～270g/L, control basicity at 40～45g/L; PH is 12.00～12.35 in control; The reaction feed liquid flows out the entering aging reactor continuously by agitated reactor top overfall, in washing press, adopt 60～65 ℃ hot deionized water wash to pH 8.00～8.50.Carry out the vacuum drier drying then, baking temperature is 80～95 ℃, obtains spherical nickel-cobalt hydroxide.
Spherical nickel-cobalt hydroxide is through joining the lithium calcining, and the lithium source is a battery-level lithium carbonate, and proportioning is a lithium carbonate: nickel cobalt hydroxide=1.08: 1, temperature are controlled at 700～900 ℃, and then obtain nickel cobalt binary material.
Adopting wet method to coat Al, is end liquid with the pure water, and nickel cobalt binary material is a base-material; Temperature is controlled at 55～70 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 25～30g/L at 80～100r/min; PH is 10.90～11.20 in control; With concentration is 70g/L aluminum sulfate solution and 18% sodium hydroxide solution, 10% ammoniacal liquor continuously and stream pump in the end liquid, the aluminum hydroxide precipitations reaction takes place and is grown in nickel cobalt binary material surface at 50～70 ℃, the gained feed liquid is after the washing and filter pressing oven dry; In 700～900 ℃ of calcinings once more, can obtain being coated with Al
2O
3Nickel cobalt binary material.
The tap density of the nickel cobalt binary material of the bag Al of preparation is 2.8～3.5g/cm
3, granularity is 5～20um.
Embodiment 5
With the pure water is end liquid, and temperature rises to 65～75 ℃.
The control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 30～40g/L at 80～120r/min, and pH is 11.50～11.70 in control.
Nickel chloride and cobalt chloride mixed solution, sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid; Nickel chloride and cobalt chloride mixed solution concentration of metal ions are 120g/L; Nickel, cobalt concentration of metal ions ratio are 6: 1, and the concentration of sodium hydroxide solution is 28%, and ammonia concn is 18%.
Precipitation reaction takes place at 65～75 ℃; Control reaction system the slip solid content 250～300g/L, control basicity at 30～40g/L; PH is 12.35～12.50 in control; The reaction feed liquid flows out the entering aging reactor continuously by agitated reactor top overfall, in washing press, adopt 65～75 ℃ hot deionized water wash to pH 7.50～8.00.Carry out the vacuum drier drying then, baking temperature is 100～120 ℃, obtains spherical nickel-cobalt hydroxide.
Spherical nickel-cobalt hydroxide is through joining the lithium calcining, and the lithium source is a battery-level lithium carbonate, and proportioning is a lithium carbonate: nickel cobalt hydroxide=1: 1, temperature are controlled at 600～750 ℃, and then obtain nickel cobalt binary material.
Adopting wet method to coat Al, is end liquid with the pure water, and nickel cobalt binary material is a base-material; Temperature is controlled at 45～60 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 20～25g/L at 80～105r/min; PH is 11.20～11.50 in control; With concentration is 60g/L aluminum sulfate solution and 24% sodium hydroxide solution, 15% ammoniacal liquor continuously and stream pump in the end liquid, the aluminum hydroxide precipitations reaction takes place and is grown in nickel cobalt binary material surface at 40～60 ℃, the gained feed liquid is after the washing and filter pressing oven dry; In 600～750 ℃ of calcinings once more, can obtain being coated with Al
2O
3Nickel cobalt binary material.
The tap density of the nickel cobalt binary material of the bag Al of preparation is 2.8～3.5g/cm
3, granularity is 5～20um.
Above content only is to be given an example and explanation to what the present invention's design did; Under the technical staff in present technique field described specific embodiment is made various modifications or replenish or adopt similar mode to substitute; Only otherwise depart from the design of invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.
Claims (9)
1. a preparation method who wraps the nickel cobalt binary material of Al is characterized in that, comprises the steps:
With the pure water is end liquid, and temperature rises to 40～80 ℃;
The control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 25～45g/L at 80～180r/min, and pH is 11.50～12.50 in control;
Nickel salt and cobalt salt mixed solution, sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid; Precipitation reaction takes place at 40～80 ℃; Slip solid content, basicity and the pH of control reaction system; The reaction feed liquid flows out the entering aging reactor continuously by agitated reactor top overfall, and is dry through washing press washing and vacuum drier, obtains spherical nickel-cobalt hydroxide;
Spherical nickel-cobalt hydroxide obtains nickel cobalt binary material through joining the lithium calcining;
Adopting wet method to coat Al, is end liquid with the pure water, and nickel cobalt binary material is a base-material; Temperature is controlled at 40～80 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree 20～40g/L at 80～160r/min; PH is 10.50～11.50 in control, aluminum sulfate solution, sodium hydroxide solution and ammoniacal liquor is also flowed continuously pump in the end liquid, the aluminum hydroxide precipitation reaction takes place and be grown in nickel cobalt binary material surface at 40～80 ℃; The gained feed liquid is calcining once more after the washing and filter pressing oven dry, can obtain being coated with Al
2O
3Nickel cobalt binary material.
2. a kind of preparation method who wraps the nickel cobalt binary material of Al according to claim 1 is characterized in that described nickel salt is nickelous sulfate, nickel chloride or nickel nitrate; Cobalt salt is cobaltous sulfate, cobalt chloride or cobalt nitrate.
3. a kind of preparation method who wraps the nickel cobalt binary material of Al according to claim 1 is characterized in that the mixed solution concentration of metal ions of described nickel salt and cobalt salt is 60～120g/L, and nickel, cobalt concentration of metal ions ratio are 2～8: 1; The concentration of described sodium hydroxide solution is 15～30%, and the concentration of ammoniacal liquor is 10～25%; The concentration of described aluminum sulfate solution is 60～100g/L.
4. a kind of preparation method who wraps the nickel cobalt binary material of Al according to claim 1; It is characterized in that in the described nickel cobalt hydroxide reaction system, basicity is controlled at 25～45g/L; The slurry solid content is controlled at 150～300g/L, and pH is 11.50～12.50 in control.
5. a kind of preparation method who wraps the nickel cobalt binary material of Al according to claim 1 is characterized in that, the washing of described spherical nickel-cobalt hydroxide adopt 50～80 ℃ hot deionized water wash to pH 7.50～9.50; Said baking temperature is 80～120 ℃.
6. a kind of preparation method who wraps the nickel cobalt binary material of Al according to claim 1 is characterized in that described lithium source is a battery-level lithium carbonate, and proportioning is a lithium carbonate: nickel cobalt hydroxide=1～1.08: 1.
7. a kind of preparation method who wraps the nickel cobalt binary material of Al according to claim 1 is characterized in that the lithium calcining heat of joining of described spherical nickel-cobalt hydroxide is controlled at 400～900 ℃.
8. a kind of preparation method who wraps the nickel cobalt binary material of Al according to claim 1 is characterized in that, the calcining heat behind the described bag A1 is controlled at 500～900 ℃.
9. according to each described a kind of preparation method who wraps the nickel cobalt binary material of Al of claim 1～8, it is characterized in that the tap density of the nickel cobalt binary material of the bag Al of preparation is 2.8～3.5g/cm
3, granularity is 5～20um.
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| CN104934594A (en) * | 2015-04-28 | 2015-09-23 | 湖南兴瑞新材料研究发展有限公司 | Coating modified nickel-cobalt binary material, and preparation method and application of material |
| CN108473338A (en) * | 2016-01-05 | 2018-08-31 | Ecopro Bm有限公司 | The manufacturing method for plating cobalt precursors, the plating cobalt precursors manufactured by the above method and the anode active material using the manufacture of above-mentioned precursor |
| CN108473338B (en) * | 2016-01-05 | 2021-05-04 | Ecopro Bm有限公司 | Method for producing cobalt plating precursor, cobalt plating precursor produced by the method, and cathode active material produced using the precursor |
| CN106654249A (en) * | 2016-04-29 | 2017-05-10 | 青岛乾运高科新材料股份有限公司 | Synthesis method for high-performance lithium-rich manganese-based positive electrode material |
| CN106067545A (en) * | 2016-07-01 | 2016-11-02 | 常州信息职业技术学院 | One sodium metaaluminate makees raw material cladding stratiform method for preparing anode material |
| CN106067545B (en) * | 2016-07-01 | 2018-07-31 | 常州信息职业技术学院 | A kind of sodium metaaluminate makees raw material cladding stratiform method for preparing anode material |
| CN106340629A (en) * | 2016-11-07 | 2017-01-18 | 珠海格力电器股份有限公司 | Modification method of lithium cobaltate material |
| CN107706368A (en) * | 2017-09-08 | 2018-02-16 | 绵阳梨坪科技有限公司 | A kind of preparation method of the nickel cobalt binary material of alclad |
| CN111430711A (en) * | 2020-03-30 | 2020-07-17 | 新乡天力锂能股份有限公司 | Coated lithium ion battery positive electrode active material and preparation method thereof |
| CN115504537A (en) * | 2022-09-27 | 2022-12-23 | 厦门厦钨新能源材料股份有限公司 | Waste liquid treatment method for wet-process coated anode material |
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