CN103178259A - Preparation method of cobalt-coated lithium ion battery anode material - Google Patents
Preparation method of cobalt-coated lithium ion battery anode material Download PDFInfo
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- CN103178259A CN103178259A CN2013100431794A CN201310043179A CN103178259A CN 103178259 A CN103178259 A CN 103178259A CN 2013100431794 A CN2013100431794 A CN 2013100431794A CN 201310043179 A CN201310043179 A CN 201310043179A CN 103178259 A CN103178259 A CN 103178259A
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Abstract
The invention discloses a preparation method of a cobalt-coated lithium ion battery anode material. The preparation method comprises the following steps of: coating Co(OH)2 on the surface of a lithium manganate matrix through chemical precipitation, wherein a complexing agent solution, a precipitant solution and a metal cobalt salt solution are added to a high-speed stirring reaction kettle, which is used for mixing up lithium manganate LiMn2O4 sizing agent, for carrying out a precipitation reaction; carrying out solid-liquid separating and drying into the discharged sizing agent after the cobalt precipitate is sufficiently reacted; carrying out high-temperature oxidation onto the materials by utilizing an oxidizing furnace under an oxygen atmosphere and a strong alkaline environment; carrying out pure water washing and solid-liquid separation onto the solid material after the oxidation reaction is completed; and obtaining the hydroxyl cobalt oxide-coated lithium manganate anode material after drying. The preparation method disclosed by the invention is low in device requirement, simple in process, good in material conductivity, long in cycle life, good in rate capability and high in capacity.
Description
Technical field
The present invention relates to a kind of coating modification method for preparing of lithium manganate material, especially coat the LiMn2O4 LiMn of cobalt
2O
4.xCoOOH preparation method.
Background technology
Lithium battery is as the environmental protection power supply of a new generation, and it has high energy density, the high advantages such as discharge platform, is widely used in 3C and the electric tool electronic products such as mobile phone, camera, notebook computer.Along with the technical development of lithium battery, require it to have the characteristics such as high-energy, high power and low cost.The positive electrode of lithium battery is the important component part of lithium battery, is the major effect factor of lithium battery performance, and present business-like positive electrode mainly contains LiCoO
2, LiMn
2O
4, Li (NixCoyMnz) O
2, Li (NixCoyALz) O
2And LiFePO
4, LiMn
2O
4Price is minimum, and fail safe is also higher, common LiMnO
4There are John-Teller effect and Mn stripping.
Lithium manganate cell positive electrode material is coated modification mainly to be comprised: coat Al
2O
3, ZnO, TiO
2, MgO, Sn O
2, CeO
2And Coated with Organic Matter, the material electric conductivity after it coats is all relatively poor, and needs high-temperature process, and easily with inner LiMn2O4 reaction, the positive electrode capacity decreases.
Summary of the invention
Problem to be solved by this invention mainly is to provide a kind of method for preparing anode material of lithium-ion battery that coats cobalt, and the doubly forthright and cycle life of positive electrode is obviously improved.
A kind of method for preparing anode material of lithium-ion battery that coats cobalt has following steps and process,
Step 1 coats,
(1) get the raw materials ready, standby cobalt salt solution, concentration of cobalt ions is 50～100g/L; Standby ammonia spirit is as complexing agent; Standby NaOH solution is as precipitation reagent;
(2) size mixing, add LiMn2O4 solution to size mixing in reactor, the solid content after the formation slurry is 150～200g/L;
(3) precipitation reaction adds complexing agent ammonia spirit, precipitation reagent NaOH solution in the reactor of existing slurry with cobalt metal salt solution and stream heating, stirring, react complete after, carry out Separation of Solid and Liquid, drying, baking temperature is 80～100 ℃, must coat Co (OH)
2LiMn2O4;
Step 2, oxidation will coat Co (OH)
2LiMn2O4 oxidation in oxidation furnace, keep alkaline environment and oxygen atmosphere, temperature is 80～95 ℃, after wash, Separation of Solid and Liquid, be drying to obtain LiMn
2O
4XCoOOH, in formula, x is molal quantity.
Further, the chlorate of cobalt salt solution preference such as cobalt, sulfate, nitrate aqueous solution.
Further, described LiMn
2O
4XCoOOH molal quantity x value preferred 1%～8%.
Further, in described precipitation reaction, the preferred 2～4mol/L of precipitation reagent NaOH solution concentration; Preferred 1～the 4mol/L of ammonia spirit preferably contains 1%～3% hydrazine hydrate; In course of reaction, the pH value is excellent 9.5～10.5, the preferred 5～20g/L of ammonium concentration, and precipitation reaction temperature preferably is controlled at 50～70 ℃, preferred 1～4h of precipitation reaction time, preferred 120～250 r/min of speed of agitator; Preferred microwave is to dry materials.
Further, in the oxidizing process of described step 2, the double helix conical mixer of the preferred internal heater of oxidation furnace, preferred 150～250 L of volume, alkaline environment is for example provided by the NaOH+LiOH mixed solution, preferred 10～the 20mol/L of OH concentration, NaOH and the preferred 1:1 of LiOH mol ratio, preferred 110～150 ℃ of NaOH+LiOH mixed solution temperature, 2～8% of the preferred LiMn2O4 quality of addition, the preferred per kilogram material of oxygen flow 0.1～0.5L/min, the preferred 0.2～1h of oxidation time; Washing is excellent to wash water pH value＜10, and dry rear material moisture＜0.1% is excellent.
The present invention has following beneficial effect:
1. carry out the coating of cobalt layer, and coat Co (OH)
2In the oxygen-proof property environment, valence stability is beneficial to and is oxidized to conductivity CoOOH preferably, coats Al
2O
3, ZnO, TiO
2, CeO
2With Coated with Organic Matter on the basis material capacity without impact, after coating, material granule is more even, sphericity is higher, coating layer can not be penetrated into granule interior, can not affect the positive electrode structure;
2. to Co (OH)
2The oxidation of coating utilizes the NaOH+LiOH mixed solution that alkaline environment is provided, and LiOH helps to slow down the loss of lithium, and high-temperature oxydation generates the CoOOH of conduction, its good stability, and anti-HF corrosion obviously improves the doubly forthright and cycle life of positive electrode;
3. LiMn
2O
4XCoOOH is the better anode material for lithium-ion batteries of a kind of conductivity, and is main because Co (OH)
2Coating is oxidized to the CoOOH of good conductivity, and after coating CoOOH, low to the treatment temperature requirement, therefore equipment requirement is decreased, simplified production procedure.
In sum, the present invention can be widely used in field of batteries, particularly the electrokinetic cell field.
Description of drawings
Shown in Figure 1 is process flow diagram of the present invention.
Shown in Figure 2 is scanning electron microscopy (SEM) figure of the embodiment of the present invention 3 gained finished products.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
1. be ready to matrix LiMn2O4 800kg, in the reactor of its input with high-speed stirred and chuck system, be mixed with pure water the LiMn2O4 slurry that solid content is 180g/L.
2. preparing 2% cobalt sulfate solution of its mole according to the amount of LiMn2O4, is the solution of 50g/L with pure water with cobaltous sulfate preparing metal ion concentration, namely takes cobaltous sulfate 13.8kg, is formulated as the 110L cobalt sulfate solution.
3. prepare the sodium hydroxide solution of 85g/L with pure water.
4. prepare ammoniacal liquor (containing 1% the hydrazine hydrate) solution of 2mol/L.
Modulate the LiMn2O4 slurry, the pH value is controlled at 10.10, ammonia concn is 5～8g/L, temperature is 55 ± 1 ℃, speed of agitator is 120r/min, by 2. solution, 3. solution, the 4. measuring pump charging simultaneously of solution, 2. the charging rate of molten cobalt sulfate solution is 1.0L/min, 3. solution, 4. the charging rate of solution is controlled by pH value and system ammonium concentration, guarantee that the reaction system ammonium concentration is 5～8g/L, system pH is controlled at 10.10～10.15, and the complete rear blowing of cobaltous sulfate reaction carries out Separation of Solid and Liquid, 85 ℃ of microwave dryings to slurry.
above-mentioned material 100kg is dropped into built-in heating and double helix conical mixer that carry out public rotation, volume is 150 L, , treat that the temperature of charge intensification remains to 90 ℃, add the alkali lye for preparing to batch mixer, open simultaneously batch mixer bottom oxygen intake valve, alkaline environment is provided by the NaOH+LiOH mixed solution, OH concentration is 15mol/L, NaOH and LiOH mol ratio are 1:1, alkali liquid temperature is 130 ℃, addition is 2.5 liters, oxygen flow is 12L/min, oxidation time is 30min, react complete rear dry to material discharging washing, wash to wash water pH＜10, baking temperature is 115 ℃, material moisture after dry＜0.1%.Finished product is the LiMn2O4 that coats 2% cobalt.
Embodiment 2:
1. be ready to matrix LiMn2O4 800kg, in the reactor of its input with high-speed stirred and chuck system, be mixed with pure water the LiMn2O4 slurry that solid content is 160g/L.
2. prepare 3% cobalt sulfate solution of its mole according to the amount of LiMn2O4, with pure water, cobaltous sulfate is prepared the solution that concentration of metal ions is 50g/L, namely take cobaltous sulfate 20.6kg, be formulated as the 160L cobalt sulfate solution.
3. prepare the sodium hydroxide solution of 100g/L with pure water.
4. prepare ammoniacal liquor (containing 1% the hydrazine hydrate) solution of 2mol/L.
Modulate the LiMn2O4 slurry, the pH value is controlled at 10.15, ammonia concn is 7～10g/L, temperature is 60 ± 1 ℃, speed of agitator is 120r/min, by 2. solution, 3. solution, the 4. measuring pump charging simultaneously of solution, 2. the charging rate of molten cobalt sulfate solution is 1.0L/min, 3. solution, 4. the charging rate of solution is controlled by pH value and system ammonium concentration, guarantee that the reaction system ammonium concentration is 7～10g/L, system pH is controlled at 10.15～10.20, and the complete rear blowing of cobaltous sulfate reaction carries out Separation of Solid and Liquid, 85 ℃ of microwave dryings to slurry.
above-mentioned material 100kg is dropped into built-in heating and double helix conical mixer that carry out public rotation, volume is 150 L, treat that the temperature of charge intensification remains to 95 ℃, add the alkali lye for preparing to batch mixer, open simultaneously batch mixer bottom oxygen intake valve, alkaline environment is provided by the NaOH+LiOH mixed solution, OH concentration is 15mol/L, NaOH and LiOH mol ratio are 1:1, alkali liquid temperature is 135 ℃, addition is 3 liters, oxygen flow is 15L/min, oxidation time is 25min, react complete rear dry to material discharging washing, wash to wash water pH＜10, baking temperature is 110 ℃, material moisture after dry＜0.1%.Finished product is the LiMn2O4 that coats 3% cobalt.
Embodiment 3:
1. be ready to matrix LiMn2O4 800kg, in the reactor of its input with high-speed stirred and chuck system, be mixed with pure water the LiMn2O4 slurry that solid content is 150g/L.
2. prepare 5% cobalt sulfate solution of its mole according to the amount of LiMn2O4, with pure water, cobaltous sulfate is prepared the solution that concentration of metal ions is 75g/L, namely take cobaltous sulfate 34.3kg, be formulated as the cobalt sulfate solution of 175L.
3. prepare the sodium hydroxide solution of 120g/L with pure water.
4. prepare ammoniacal liquor (containing 1.5% the hydrazine hydrate) solution of 2.5mol/L.
Modulate the LiMn2O4 slurry, the pH value is controlled at 10.10, ammonia concn is 8～10g/L, temperature is 62 ± 1 ℃, speed of agitator is 120r/min, by 2. solution, 3. solution, the 4. measuring pump charging simultaneously of solution, 2. the charging rate of molten cobalt sulfate solution is 1.0L/min, 3. solution, 4. the charging rate of solution is controlled by pH value and system ammonium concentration, guarantee that the reaction system ammonium concentration is 8～10g/L, system pH is controlled at 10.10～10.15, and the complete rear blowing of cobaltous sulfate reaction carries out Separation of Solid and Liquid, 85 ℃ of microwave dryings to slurry.
above-mentioned material 100kg is dropped into built-in heating and double helix conical mixer that carry out public rotation, volume is 150 L, , treat that the temperature of charge intensification remains to 92 ℃, add the alkali lye for preparing to batch mixer, open simultaneously batch mixer bottom oxygen intake valve, alkaline environment is provided by the NaOH+LiOH mixed solution, OH concentration is 15mol/L, NaOH and LiOH mol ratio are 1:1, alkali liquid temperature is 125 ℃, addition is 3.5 liters, oxygen flow is 10L/min, oxidation time is 30min, react complete rear dry to material discharging washing, wash to wash water pH＜10, baking temperature is 105 ℃, material moisture＜0.1%.Finished product is the LiMn2O4 that coats 5% cobalt.
Embodiment 4:
1. be ready to matrix LiMn2O4 800kg, in the reactor of its input with high-speed stirred and chuck system, be mixed with pure water the slurry that solid content is 200g/L.
2. prepare 6% cobalt sulfate solution of its mole according to the amount of LiMn2O4, with pure water, cobaltous sulfate is prepared the solution that concentration of metal ions is 75g/L, namely take cobaltous sulfate 41.2kg, be formulated as 210L solution.
3. prepare the sodium hydroxide solution of 150g/L with pure water.
4. prepare ammoniacal liquor (containing 1.5% the hydrazine hydrate) solution of 3mol/L.
Modulate the LiMn2O4 slurry, the pH value is controlled at 10.25, ammonia concn is 8～10g/L, temperature is 65 ± 1 ℃, speed of agitator is 150r/min, by 2. solution, 3. solution, the 4. measuring pump charging simultaneously of solution, 2. the charging rate of molten cobalt sulfate solution is 1.2L/min, 3. solution, 4. the charging rate of solution is controlled by pH value and system ammonium concentration, guarantee that the reaction system ammonium concentration is 8～10g/L, system pH is controlled at 10.25～10.30, and the complete rear blowing of cobaltous sulfate reaction carries out Separation of Solid and Liquid, 85 ℃ of microwave dryings to slurry.
above-mentioned material 100kg is dropped into built-in heating and double helix conical mixer that carry out public rotation, volume is 150 L, treat that the temperature of charge intensification remains to 90 ℃, add the alkali lye for preparing to batch mixer, open simultaneously batch mixer bottom oxygen intake valve, alkaline environment is provided by the NaOH+LiOH mixed solution, OH concentration is 18mol/L, NaOH and LiOH mol ratio are 1:1, alkali liquid temperature is 120 ℃, addition is 4 liters, oxygen flow is 18L/min, oxidation time is 40min, react complete rear dry to material discharging washing, wash to wash water pH＜10, baking temperature is 110 ℃, material moisture＜0.1%.Finished product is the LiMn2O4 that coats 6% cobalt.
Embodiment 5:
1. be ready to matrix LiMn2O4 800kg, in the reactor of its input with high-speed stirred and chuck system, be mixed with pure water the slurry that solid content is 200g/L.
2. prepare 7% cobalt sulfate solution of its mole according to the amount of LiMn2O4, with pure water, cobaltous sulfate is prepared the solution that concentration of metal ions is 100g/L, namely take cobaltous sulfate 48.1kg, be formulated as 190L solution.
3. prepare the sodium hydroxide solution of 150g/L with pure water.
4. prepare ammoniacal liquor (containing 2% the hydrazine hydrate) solution of 3mol/L.
Modulate the LiMn2O4 slurry, the pH value is controlled at 10.25, ammonia concn is 8～10g/L, temperature is 65 ± 1 ℃, speed of agitator is 150r/min, by 2. solution, 3. solution, the 4. measuring pump charging simultaneously of solution, 2. the charging rate of molten cobalt sulfate solution is 1.5L/min, 3. solution, 4. the charging rate of solution is controlled by pH value and system ammonium concentration, guarantee that the reaction system ammonium concentration is 8～10g/L, system pH is controlled at 10.25～10.30, and the complete rear blowing of cobaltous sulfate reaction carries out Separation of Solid and Liquid, 85 ℃ of microwave dryings to slurry.
above-mentioned material 100kg is dropped into built-in heating and double helix conical mixer that carry out public rotation, volume is 150 L, treat that the temperature of charge intensification remains to 95 ℃, add the alkali lye for preparing to batch mixer, open simultaneously batch mixer bottom oxygen intake valve, alkaline environment is provided by the NaOH+LiOH mixed solution, OH concentration is 15mol/L, NaOH and LiOH mol ratio are 1:1, alkali liquid temperature is 135 ℃, addition is 4 liters, oxygen flow is 18L/min, oxidation time is 40min, react complete rear dry to material discharging washing, wash to wash water pH＜10, baking temperature is 110 ℃, material moisture＜0.1%.Finished product is the LiMn2O4 that coats 7% cobalt.
Claims (5)
1. a method for preparing anode material of lithium-ion battery that coats cobalt, is characterized in that, has following steps and process,
Step 1 coats,
(1) get the raw materials ready, standby cobalt salt solution, concentration of cobalt ions is 50～100g/L; Standby ammonia spirit is as complexing agent; Standby NaOH solution is as precipitation reagent;
(2) size mixing, add LiMn2O4 to size mixing in reactor, forming solid content is the slurry of 150～200g/L;
(3) precipitation reaction adds complexing agent ammonia spirit, precipitation reagent NaOH solution and cobalt salt solution and stream in the reactor of existing slurry, heating, stirs, react complete after, carry out Separation of Solid and Liquid, drying, must coat Co (OH)
2LiMn2O4;
Step 2, oxidation will coat Co (OH)
2Lithium manganate material oxidation in oxidation furnace, keep alkaline environment and oxygen atmosphere, temperature is 80～95 ℃, after wash, Separation of Solid and Liquid, drying, baking temperature is 100～150 ℃, namely gets LiMn
2O
4XCoOOH, in formula, x is molal quantity.
2. a kind of method for preparing anode material of lithium-ion battery that coats cobalt according to claim 1, is characterized in that, cobalt salt solution comprises chlorate, sulfate, the nitrate aqueous solution of cobalt.
3. a kind of method for preparing anode material of lithium-ion battery that coats cobalt according to claim 1, is characterized in that described LiMn
2O
4XCoOOH molal quantity x value is 1%～8%.
4. a kind of method for preparing anode material of lithium-ion battery that coats cobalt according to claim 1, is characterized in that, in described precipitation reaction, precipitation reagent NaOH solution concentration is 2～4mol/L; Ammonia spirit is 1～4mol/L, contains 1%～3% hydrazine hydrate; In the precipitation reaction process, the pH value is 9.5～10.5, and ammonium concentration is 5～20g/L, and precipitation reaction temperature is controlled at 50～70 ℃, and precipitation reaction time 1～4h, speed of agitator are 120～250 r/min.
5. a kind of method for preparing anode material of lithium-ion battery that coats cobalt according to claim 1, it is characterized in that, in the oxidizing process of described step 2, oxidation furnace is the double helix conical mixer of internal heater, volume is 150～250 L, alkaline environment is provided by the NaOH+LiOH mixed solution, OH concentration is 10～20mol/L, NaOH and LiOH mol ratio are 1:1, NaOH+LiOH mixed solution temperature is 110～150 ℃, addition is 2～8% of LiMn2O4 quality, oxygen flow is per kilogram material 0.1～0.5L/min, oxidation time is 0.2～1h, wash to wash water pH＜10 dry rear material moisture＜0.1%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103762379A (en) * | 2014-01-28 | 2014-04-30 | 泉州劲鑫电子有限公司 | High-capacity lithium ion battery and production process thereof |
| CN104282902A (en) * | 2014-10-20 | 2015-01-14 | 安徽师范大学 | Lithium manganate of core-shell structure and preparation method of lithium manganate |
| CN113620354A (en) * | 2021-08-06 | 2021-11-09 | 湖南杉杉能源科技有限公司 | Surface-coated lithium ion battery anode material precursor and preparation method thereof |
| CN114105216A (en) * | 2021-10-27 | 2022-03-01 | 厦门厦钨新能源材料股份有限公司 | Cobalt hydroxide with micro-crack structure, and preparation method and application thereof |
| CN114162880A (en) * | 2021-11-22 | 2022-03-11 | 宁夏中色金辉新能源有限公司 | Lithium ion solid-state battery positive active material precursor and preparation method and application thereof |
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| CN114105216B (en) * | 2021-10-27 | 2024-03-29 | 厦门厦钨新能源材料股份有限公司 | Cobalt hydroxide with micro-crack structure, and preparation method and application thereof |
| CN114162880A (en) * | 2021-11-22 | 2022-03-11 | 宁夏中色金辉新能源有限公司 | Lithium ion solid-state battery positive active material precursor and preparation method and application thereof |
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Application publication date: 20130626 |