CN107331859B - Method for rapidly synthesizing ternary lithium battery positive electrode material precursor by single kettle - Google Patents
Method for rapidly synthesizing ternary lithium battery positive electrode material precursor by single kettle Download PDFInfo
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- CN107331859B CN107331859B CN201710633152.9A CN201710633152A CN107331859B CN 107331859 B CN107331859 B CN 107331859B CN 201710633152 A CN201710633152 A CN 201710633152A CN 107331859 B CN107331859 B CN 107331859B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the field of battery material manufacturing, and particularly relates to a method for rapidly synthesizing a ternary lithium battery anode material precursor by a single kettle. Feeding into the reaction kettle, enabling the liquid level in the reaction kettle to rise to an overflow port, then enabling the slurry to overflow into the thickener, connecting the bottom of the thickener with a circulating pump, and enabling the outlet of the circulating pump to be located in the reaction kettle and used for pumping the slurry in the thickener back into the reaction kettle. The filter rods of the filtering part in the thickener are regularly arranged and collected to be connected to the vacuum buffer tank, part of slurry is filtered by the filter rods, particles in the slurry are intercepted in the thickener, the concentrated slurry is pumped back to the reaction kettle through the circulating pump to continue reaction, and the filtrate passing through the filter rods is discharged into the vacuum buffer tank. The invention can enhance the thickening effect, greatly improve the flow of the synthesized ternary liquid, accelerate the reaction speed and improve the yield of the synthesis stage, thereby improving the yield and reducing the cost.
Description
Technical Field
The invention belongs to the field of battery material manufacturing, and particularly relates to a method for rapidly synthesizing a ternary lithium battery anode material precursor by a single kettle.
Background
The nickel-cobalt-manganese hydroxide is a precursor of a positive electrode material of a ternary finished battery (nickel-cobalt-manganese lithium manganate), and the ternary lithium polymer battery has the advantages of low cost, high gram capacity (more than 150mAh/g), working voltage matched with the conventional electrolyte, high safety, excellent cyclicity, high gram capacity and the like. The method is widely applied to the fields of small-sized electric appliances, electric tools, electric automobiles and the like. The nickel-cobalt-manganese hydroxide synthesis process mostly adopts an independent reaction kettle for reaction, materials before the particle size reaches the standard directly overflow from an overflow port in the reaction process to become unqualified products, and the unqualified products can be obtained only after the materials overflow until the particle size in the kettle is qualified. The simple dense groove is gradually manufactured by a manufacturer and connected with the reaction kettle, so that materials overflow from the simple dense groove, the dense groove has no stirring, the effect of settling particles can be achieved, the particle loss can be reduced, the solid content in the reaction kettle can be properly improved, the yield of the method is still poor, and the reaction time is long.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for rapidly synthesizing a precursor of a ternary lithium battery anode material by a single kettle.
The rapid synthesis device related to the method comprises a reaction kettle and a thickener, wherein an overflow port is arranged on the reaction kettle and is communicated with the thickener, the bottom of the thickener is connected with the reaction kettle through a circulating pump, a filter stick is arranged in the thickener, and mother liquor passing through the filter stick is collected and then is connected with a vacuum buffer tank through a flowmeter and a pneumatic valve.
Preferably, the bottom of the reaction kettle is connected with the top of the thickener through a centrifugal pump.
the synthesis process is as follows:
1) Feeding the ternary nickel-cobalt-manganese solution, the NaOH solution and the ammonia water into a reaction kettle at a constant speed through a flowmeter, controlling the temperature in the reaction kettle at 40-70 ℃ and the pH at 10.0-12.0, and when the liquid level of the reaction kettle reaches an overflow port, overflowing the slurry in the reaction kettle into a thickener;
2) When the liquid level meter of the thickener displays the liquid level H 1 m, the thickener control system starts a stirring motor, when the liquid level of the thickener reaches H 2 m, the pneumatic valve is started by the thickener control system, the vacuum buffer tank is communicated with the thickener at the moment, the vacuum buffer tank pumps the mother liquor passing through the filter stick out of the thickener through negative pressure, when the liquid level in the thickener reaches H 3 m, the pneumatic valve is closed, the mother liquor pumping is stopped, H 1 is more than H 3 and more than H 2, and the slurry in the thickener is continuously pumped into the reaction kettle by a circulating pump at the bottom of the thickener for circulation;
3) When the particle size of solid particles reaches 9.0-20um through sampling detection in the reaction kettle, the particle size is qualified, the feeding is stopped, and the synthesis is finished.
In the step 2), the frequency f =10-50Hz of the stirring motor of the thickener.
in the step 2), the vacuum degree of the vacuum buffer tank is controlled at 20 ~ 80 KPa.
As an example, the synthesis procedure is as follows:
1) Feeding 80-120g/L of nickel-cobalt-manganese ternary solution, 30-34wt% of NaOH solution and 12-18wt% of ammonia water into a 6.0-8.0 m-thin-film reaction kettle at constant speed through a mass flow meter, controlling the flow of the ternary solution at 600-1200L/h, controlling the temperature in the reaction kettle at 50-70 ℃ and the pH at 10.0-11.0, and when the liquid level of the reaction kettle reaches an overflow port, overflowing the slurry in the reaction kettle to a thickener with the volume of 3.7 m;
2) When the liquid level meter of the thickener displays that the liquid level is 0.4m, the thickener control system starts a stirring motor, when the liquid level of the thickener reaches 1.0m, the thickener control system starts a pneumatic valve, at the moment, a vacuum buffer tank is communicated with the thickener, the vacuum buffer tank pumps the mother liquor passing through the filter stick out of the thickener through negative pressure, when the liquid level in the thickener reaches 0.8m, a pneumatic valve is closed, the mother liquor pumping is stopped, and a circulating pump at the bottom of the thickener continuously pumps the slurry in the thickener into a reaction kettle for circulation;
3) When the particle size of solid particles reaches 9-20um through sampling detection in the reaction kettle, the particle size is qualified, the feeding is stopped, and the synthesis is finished.
In the rapid synthesis device, the filter stick in the thickener is provided with a nitrogen pipe and a pure water pipe for back flushing regeneration of the filter stick.
The reaction kettle is also provided with a temperature measuring instrument and a pH meter.
The thickener is also provided with a liquid level meter.
When the ternary precursor is prepared, feeding the ternary precursor into a reaction kettle, enabling the slurry to overflow into a thickener after the liquid level in the reaction kettle rises to an overflow port, connecting the bottom of the thickener with a circulating pump, and enabling an outlet of the circulating pump to be arranged in the reaction kettle and be used for pumping the slurry in the thickener back into the reaction kettle. Filter rods of a filtering part in the thickener are regularly arranged and gathered to be connected to a vacuum buffer tank, particles in the slurry are intercepted in the thickener after the partial slurry is filtered by the filter rods, the concentrated slurry is pumped back to the reaction kettle through a circulating pump to continue reaction, filtrate passing through the filter rods is discharged into the vacuum buffer tank, the vacuum buffer tank is communicated with a vacuum pump, the vacuum pump continuously operates to ensure a negative pressure environment in the buffer tank, and the operation of pumping and filtering liquid in the thickener is continuously carried out. And discharging the filtrate accumulated in the vacuum buffer tank to a filtrate storage tank after obtaining a certain liquid level, and then discharging after further treatment. If the vacuum negative pressure system fails, the mother liquor can be discharged in a positive pressure filter pressing mode through a pump connected with the lower portion of the reaction kettle to a pipeline at the top of the thickener.
aiming at the problems of slow growth speed, low yield and the like of the nickel-cobalt-manganese hydroxide ternary precursor in the synthesis stage, the invention can enhance the thickening effect, greatly improve the flow of the synthesized ternary liquid, accelerate the reaction speed and improve the yield in the synthesis stage, thereby improving the yield and reducing the cost.
Drawings
FIG. 1 is a schematic structural diagram of a rapid synthesis apparatus for a precursor of a ternary lithium battery cathode material, wherein 1-an overflow port; 2-a reaction kettle; 3-a densifier; 4-a vacuum pump; 5-a circulating pump; 6-stirring a motor; 7-a liquid level meter; 8-vacuum buffer tank; 9-filtering the filter stick; 10-pneumatic valves; 11-a flow meter; 12-centrifugal pump.
Detailed Description
as shown in figure 1, the rapid synthesis device related to the method comprises a reaction kettle and a thickener, wherein an overflow port is arranged on the reaction kettle and is communicated with the thickener, the bottom of the thickener is connected with the reaction kettle through a circulating pump, a filter stick is arranged in the thickener, and mother liquor passing through the filter stick is collected and then is connected with a vacuum buffer tank through a flowmeter and a pneumatic valve.
50When the specific implementation is carried out, feeding is carried out in a reaction kettle, slurry overflows into a thickener after the liquid level in the reaction kettle rises to an overflow port, 70-120g/L of nickel-cobalt-manganese ternary solution with the concentration, 15-40% of NaOH solution and 5-25% of ammonia water are simultaneously fed into the reaction kettle through a flowmeter at a constant speed, the flow rate of the ternary solution is controlled at 1200L/h, the pH value in the reaction kettle is detected to be 10.0-12.0 by sampling, the ammonia concentration in supernatant is 2.0-12.0g/L, a temperature instrument on the reaction kettle automatically controls the temperature to be 40-70 ℃, when the liquid level of the reaction kettle reaches the joint of the reaction kettle and the thickener by sampling, the liquid level in the reaction kettle overflows into the thickener, when the liquid level meter of the thickener shows that the liquid level is 0.4m, the thickener automatic control system automatically starts the thickener stirring (f =10-50 Hz) when the liquid level meter shows that the liquid level is 0.4m, the stirring in the reaction kettle continuously operates, when the liquid level of the thickener reaches 1m, the automatic control system automatically starts the thickener, the vacuum buffer tank automatically starts the stirring (f =10-50 Hz), the vacuum degree control the vacuum buffer tank is communicated with the thickener, the mother liquor, the vacuum buffer tank, the vacuum valve stops the vacuum valve is communicated with the mother liquor when the concentration synthesis process of the concentration synthesis tank, the vacuum buffer tank, the vacuum synthesis tank is communicated with the vacuum buffer tank, the vacuum synthesis tank.
In the production process, the mother liquor is discharged through negative pressure after passing through a high-precision filter stick in the thickener, solid particles are left in a cavity of the thickener, the slurry in the thickener can be in a uniform state through stirring in the thickener, and the concentrated slurry in the thickener is pumped into a normal reaction system in the reaction kettle for continuous reaction through a circulating pump at the bottom of the thickener until a qualified precursor product is synthesized. The large filtering area of the thickener can finish the feeding amount of the large metal solution of the reaction system, can improve the reaction rate and improve the production efficiency. The high-precision filter stick of the thickener can finish mother liquor discharge and solid particle interception, completely solves the problem of overflow material waste before the indexes in the reaction kettle are unqualified in the reaction process, and greatly improves the yield and the unit yield.
Claims (7)
1. A method for rapidly synthesizing a ternary lithium battery anode material precursor by a single kettle is characterized in that a used synthesizing device comprises a reaction kettle and a thickener, wherein an overflow port is formed in the reaction kettle and is communicated with the thickener, the bottom of the thickener is connected with the reaction kettle through a circulating pump, a filter rod is arranged in the thickener, and mother liquor passing through the filter rod is collected and then is connected with a vacuum buffer tank through a flowmeter and a pneumatic valve;
The synthesis process is as follows:
1) Feeding the ternary nickel-cobalt-manganese solution, the NaOH solution and the ammonia water into a reaction kettle at a constant speed through a flowmeter, controlling the temperature in the reaction kettle at 40-70 ℃ and the pH at 10.0-12.0, and when the liquid level of the reaction kettle reaches an overflow port, overflowing the slurry in the reaction kettle into a thickener;
2) When the liquid level meter of the thickener displays the liquid level H 1 m, the thickener control system starts a stirring motor, when the liquid level of the thickener reaches H 2 m, the pneumatic valve is started by the thickener control system, the vacuum buffer tank is communicated with the thickener at the moment, the vacuum buffer tank pumps the mother liquor passing through the filter stick out of the thickener through negative pressure, when the liquid level in the thickener reaches H 3 m, the pneumatic valve is closed, the mother liquor pumping is stopped, H 1 is more than H 3 and more than H 2, and the slurry in the thickener is continuously pumped into the reaction kettle by a circulating pump at the bottom of the thickener for circulation;
3) When the particle size of solid particles reaches 9.0-20um through sampling detection in the reaction kettle, the particle size is qualified, the feeding is stopped, and the synthesis is finished.
2. The method of claim 1, wherein the synthesis process is as follows:
1) feeding 80-120g/L of nickel-cobalt-manganese ternary solution, 30-34wt% of NaOH solution and 12-18wt% of ammonia water into a 6.0-8.0 m-thin-film reaction kettle at constant speed through a mass flow meter, controlling the flow of the ternary solution at 600-1200L/h, controlling the temperature in the reaction kettle at 50-70 ℃ and the pH at 10.0-11.0, and when the liquid level of the reaction kettle reaches an overflow port, overflowing the slurry in the reaction kettle to a thickener with the volume of 3.7 m;
2) When the liquid level meter of the thickener displays that the liquid level is 0.4m, the thickener control system starts a stirring motor, when the liquid level of the thickener reaches 1.0m, the thickener control system starts a pneumatic valve, at the moment, a vacuum buffer tank is communicated with the thickener, the vacuum buffer tank pumps the mother liquor passing through the filter stick out of the thickener through negative pressure, when the liquid level in the thickener reaches 0.8m, a pneumatic valve is closed, the mother liquor pumping is stopped, and a circulating pump at the bottom of the thickener continuously pumps the slurry in the thickener into a reaction kettle for circulation;
3) When the particle size of solid particles reaches 9-20um through sampling detection in the reaction kettle, the particle size is qualified, the feeding is stopped, and the synthesis is finished.
3. The method according to claim 1 or 2, characterized in that in step 2) the frequency f =10-50Hz of the stirring motor of the thickener.
4. the method according to claim 1 or 2, wherein in step 2), the vacuum degree of the vacuum buffer tank is controlled at 20 ~ 80 KPa.
5. The method according to claim 1 or 2, wherein in the synthesizing device, the filter stick in the thickener is provided with a nitrogen pipe and a pure water pipe for filter stick blowback regeneration.
6. The method according to claim 1 or 2, wherein the reaction kettle is further provided with a temperature measuring instrument and a pH meter in the synthesis device.
7. The method according to claim 1 or 2, wherein the synthesizer further comprises a liquid level meter in the densifier.
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| CN107857309A (en) * | 2017-11-16 | 2018-03-30 | 湖南中伟新能源科技有限公司 | A kind of preparation method of continous way nickel-cobalt-manganese ternary presoma |
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| CN111072076A (en) * | 2019-06-28 | 2020-04-28 | 当升科技(常州)新材料有限公司 | Positive electrode material precursor preparation device and positive electrode material precursor preparation method |
| CN112713269B (en) * | 2020-12-31 | 2021-10-29 | 浙江帕瓦新能源股份有限公司 | Production system and production method for reducing content of sodium ions and sulfate ions in precursor of positive electrode material |
| CN114014383A (en) * | 2021-11-05 | 2022-02-08 | 广东佳纳能源科技有限公司 | High-tap-density positive electrode material and preparation method of positive electrode piece |
| CN114733464B (en) * | 2022-04-18 | 2024-03-22 | 成都思达能环保设备有限公司 | Positive electrode material precursor coprecipitation reaction system |
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Effective date of registration: 20221130 Address after: 448124 No. 3, Yingchun Avenue, Duodao District, High tech Zone, Jingmen City, Hubei Province Patentee after: JINGMEN GEM Co.,Ltd. Patentee after: Fu'an Qingmei Energy Materials Co.,Ltd. Address before: 448124 high tech Industrial Development Zone, Jingmen City, Hubei Province Patentee before: JINGMEN GEM Co.,Ltd. |