CN107308898B - Rapid synthesis device for ternary lithium battery anode material precursor - Google Patents

Rapid synthesis device for ternary lithium battery anode material precursor Download PDF

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Publication number
CN107308898B
CN107308898B CN201710632162.0A CN201710632162A CN107308898B CN 107308898 B CN107308898 B CN 107308898B CN 201710632162 A CN201710632162 A CN 201710632162A CN 107308898 B CN107308898 B CN 107308898B
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thickener
buffer tank
reaction kettle
pump
vacuum buffer
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CN107308898A (en
Inventor
许开华
乐绪清
李涛
白亮
陈天斌
唐兴邦
吕志
李友福
杨开
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Gem Jiangsu Cobalt Industry Co Ltd
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Gem Jiangsu Cobalt Industry Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B01D36/04—Combinations of filters with settling tanks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
    • 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
    • H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention belongs to the field of battery material manufacturing, and particularly relates to a rapid synthesis device for a ternary lithium battery anode material precursor. The reaction kettle is provided with an overflow port, the overflow port 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, mother liquor passing through the filter rod is collected and then connected with a vacuum buffer tank through a flowmeter and a pneumatic valve, the upper part of the vacuum buffer tank is connected with a vacuum pump, and the bottom of the vacuum buffer tank is connected with a mother liquor storage tank. The device can play a role in enhancing the thickening effect, greatly improving the synthesized ternary flow, accelerating the reaction speed and improving the yield of the synthesis stage, thereby improving the yield and reducing the cost.

Description

Rapid synthesis device for ternary lithium battery anode material precursor
Technical Field
The invention belongs to the field of battery material manufacturing, and particularly relates to a rapid synthesis device for a ternary lithium battery anode material precursor.
Background
The nickel cobalt manganese hydroxide is a positive electrode material precursor of a ternary finished battery (nickel cobalt lithium manganate), and the ternary lithium polymer battery has the advantages of low cost, high gram capacity (150 mAh/g), good safety, excellent circularity, high gram capacity and the like, and the working voltage is matched with the existing electrolyte. The method is widely applied to the fields of small-sized electric appliances, electric tools, electric automobiles and the like. In the process of synthesizing nickel cobalt manganese hydroxide, an independent reaction kettle is adopted for reaction, and before the particle size does not reach the standard in the reaction process, materials directly overflow from an overflow port to become unqualified products until the particle size in the kettle is qualified. The simple and dense tank is manufactured by a manufacturer gradually and is connected with the reaction kettle, so that materials overflow from the simple and dense tank, the dense tank is not stirred, 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, but the yield of the method is still poor, and the reaction time is long.
Disclosure of Invention
The invention aims to provide a rapid synthesis device for a ternary lithium battery anode material precursor.
The utility model provides a quick synthesizer of ternary lithium cell positive electrode material precursor, includes reation kettle and concentrator, there is the overflow mouth on the reation kettle, overflow mouth and concentrator intercommunication, the concentrator bottom links to each other with reation kettle through the circulating pump, there is the filter rod in the concentrator, the mother liquor through the filter rod is summarized the back and is connected vacuum buffer tank through flowmeter, pneumatic valve, vacuum buffer tank upper portion is connected with the vacuum pump, and the bottom is connected with the mother liquor storage tank.
Preferably, the bottom of the reaction kettle is also connected with the top of the thickener through a centrifugal pump.
When the ternary precursor is prepared, feeding is carried out in the reaction kettle, slurry overflows into the thickener after the liquid level in the reaction kettle rises to the overflow port, the bottom of the thickener is connected with the circulating pump, and the outlet of the circulating pump is connected into the reaction kettle and is 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 are summarized and connected to the 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 by the circulating pump to continue to react, mother liquor passing through the filter rods is discharged into the vacuum buffer tank, the vacuum buffer tank is communicated with the vacuum pump, the vacuum pump continuously operates to ensure the negative pressure environment in the buffer tank, and the mother liquor pumping operation is continuously carried out in the thickener. The accumulated mother liquor in the vacuum buffer tank is discharged to a mother liquor storage tank after a certain liquid level is obtained, and then is discharged after further treatment.
The filter stick in the thickener is provided with a nitrogen pipe and a pure water pipe for back blowing regeneration of the filter stick.
The reaction kettle is also provided with a thermometer and a pH meter.
The thickener is also provided with a liquid level meter.
Aiming at the problems of low growth speed, low yield and the like of the cobalt nickel manganese hydroxide ternary precursor in the synthesis stage, the invention can play a role in enhancing the thickening effect, greatly improving the ternary flow rate of synthesis, accelerating the reaction speed, improving 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 device for ternary lithium battery positive electrode material precursors, wherein the rapid synthesis device comprises a 1-overflow port; 2-a reaction kettle; 3-densifier; 4-a vacuum pump; 5-a circulation pump; 6, a stirring motor; 7-a liquid level meter; 8-a vacuum buffer tank; 9-a filter stick; 10-a pneumatic valve; 11-a flow meter; 12-centrifugal pump.
Detailed Description
As shown in figure 1, the rapid synthesis device for the ternary lithium battery anode material precursor comprises a reaction kettle and a thickener, wherein an overflow port is formed in the reaction kettle, the overflow port 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, filtrate passing through the filter rod is collected and then is connected with a vacuum buffer tank through a flowmeter and a pneumatic valve, the upper part of the vacuum buffer tank is connected with a vacuum pump, and the bottom of the vacuum buffer tank is connected with a filtrate storage tank.
When the negative pressure system of the thickener fails, the reaction kettle can be started to the pump of the thickener, and the slurry in the kettle is pumped into the thickener through the pump to carry out positive pressure filter pressing.
In the concrete implementation, the material is fed into the reaction kettle, and the slurry overflows into the thickener after the liquid level in the reaction kettle rises to an overflow port. 70-120g/L of nickel-cobalt-manganese ternary liquid, 15-40wt% of NaOH solution and 5-25wt% of ammonia water are simultaneously fed into a reaction kettle at a constant speed through a flowmeter, the flow rate of the ternary liquid is controlled at 300-1500L/h, the pH value in the reaction kettle is controlled at 10.0-12.0 by sampling and detecting, the ammonia concentration in the supernatant is 2.0-12.0g/L, and the temperature of a thermometer on the reaction kettle is automatically controlled at 40-70 ℃. When the liquid level of the reaction kettle reaches the joint of the reaction kettle and the thickener, the liquid level in the reaction kettle overflows into the thickener with the volume of 0.5-6.0m, and when the liquid level gauge of the thickener displays the liquid level H 1 And (3) automatically starting the thickener stirring (f=10-50 Hz) by an automatic control system of the thickener in the m time, and continuously operating the thickener stirring in the reaction process until the material is discharged after the reaction is stopped qualified. When the liquid level of the thickener reaches H 2 m, opening a mother liquor discharging pneumatic valve, at the moment, controlling the vacuum buffer tank (the vacuum degree is controlled at 20-80 KPa) to be communicated with the thickener, and pumping the mother liquor in the thickener out of the thickener through negative pressure by the vacuum buffer tank, and when the liquid level in the thickener reaches H 3 And (m) automatically closing the mother liquor discharging pneumatic valve to stop mother liquor pumping. H 1 <H 3 <H 2 . If the negative pressure system of the thickener fails in the process, a centrifugal pump at the bottom of the reaction kettle can be started, slurry in the kettle is pumped into the thickener through the pump, and mother liquor is discharged through pressure filtration by positive pressure. The circulation is that the particle size is sampled and detected from the reaction kettle to D in the synthesis process 50 When the particle size is qualified when the particle size is 9.0-20.0um, stopping feeding and completing the synthesis. Compared with the traditional mode, the reaction time is 100-150% shorter, and the yield can be improved to 99%.
In the production process, mother liquor is discharged through negative pressure after passing through a high-precision filter rod in a thickener, solid particles are left in a thickener cavity, slurry in the thickener is in a uniform state due to stirring in the thickener, concentrated slurry in the thickener is pumped into a normal reaction system in a reaction kettle through a circulating pump at the bottom of the thickener to continue to react until a qualified precursor product is synthesized, if a negative pressure system of the thickener fails in the process, the reaction kettle can be started to a thickener pump, the slurry in the kettle is pumped into the thickener through the pump, and mother liquor is discharged through pressure filtration. The same system can finish the multifunctional operation with negative pressure suction filtration as the main part and positive pressure filtration as the auxiliary part. The large filtering area of the thickener can complete the feeding amount of the large metal solution of the reaction system, can improve the reaction rate and the production efficiency. The high-precision filter stick of the thickener can be used for completing mother liquor discharge to intercept solid particles, so that the problem of waste of overflow materials before indexes in a reaction kettle are unqualified in the reaction process is completely solved, and the yield and unit yield are greatly improved.

Claims (4)

1. A rapid synthesis method of ternary lithium battery anode material precursor, the device used comprises a reaction kettle and a thickening device
The reactor is provided with an overflow port, the overflow port is communicated with the thickener, and the bottom of the thickener is communicated with the reactor through a circulating pump
The thickener is internally provided with a filter stick, mother solution passing through the filter stick is collected and then is connected with a vacuum buffer tank through a flowmeter and a pneumatic valve, and the filter stick is connected with a vacuum buffer tank through a pressure sensor
The upper part of the vacuum buffer tank is connected with a vacuum pump, the bottom of the vacuum buffer tank is connected with a mother liquor storage tank, and the bottom of the reaction kettle is also connected with a centrifugal pump
The top of the thickener is connected, and the synthesis method comprises the following steps:
feeding into a reaction kettle, overflowing slurry 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, discharging the circulating pump into the reaction kettle, regularly arranging filter rods of a filtering part in the thickener, collecting and connecting the filter rods to a vacuum buffer tank, filtering part of slurry by the filter rods, intercepting particles in the slurry in the thickener, pumping the concentrated slurry back into the reaction kettle through the circulating pump for continuous reaction, discharging mother liquor passing through the filter rods into the vacuum buffer tank, communicating the vacuum buffer tank with the vacuum pump, and continuously operating the vacuum pump to ensure a negative pressure environment in the buffer tank and continuously performing mother liquor pumping operation on the inside of the thickener; if the negative pressure system of the thickener fails in the process, starting the reaction kettle to the pump of the thickener, pumping the slurry in the kettle into the thickener through the pump, and carrying out pressure filtration to discharge mother liquor through positive pressure.
2. The rapid synthesis method according to claim 1, wherein the filter rod in the thickener comprises a nitrogen pipe and a nitrogen pipe
The pure water pipe is used for back blowing regeneration of the filter stick.
3. The rapid synthesis method according to claim 1, wherein the reaction vessel is further equipped with a thermometer and pH
And (5) counting.
4. The rapid synthesis process according to claim 1, wherein the densifier is further equipped with a level gauge.
CN201710632162.0A 2017-07-28 2017-07-28 Rapid synthesis device for ternary lithium battery anode material precursor Active CN107308898B (en)

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CN109896553A (en) * 2017-12-11 2019-06-18 河南科隆新能源股份有限公司 A kind of preparation method for the ball-shape nickel hydroxide cobalt manganese presoma that particle diameter distribution is narrow
CN109985597A (en) * 2018-01-02 2019-07-09 上海亚洲化学品有限公司 A kind of energy-efficient liquid phase mixture reaction unit
CN109160545B (en) * 2018-07-24 2021-01-05 格林美股份有限公司 Nickel cobalt lithium manganate precursor synthesizer
CN110723758A (en) * 2018-12-25 2020-01-24 北京当升材料科技股份有限公司 Lithium battery positive electrode material precursor synthesis device and method
CN110102232A (en) * 2019-05-23 2019-08-09 傅荣华 Concentration systems are used in a kind of production of lithium battery persursor material
CN111111590B (en) * 2019-12-27 2022-04-22 苏州清陶新能源科技有限公司 Method for stirring anode slurry
CN112209451B (en) * 2020-10-10 2023-03-28 中国科学院宁波材料技术与工程研究所 Multi-stage reaction system, lithium ion multi-element anode material precursor and preparation method thereof, and preparation method of lithium ion multi-element anode material
CN113750946B (en) * 2021-10-22 2023-12-22 上海安赐环保科技股份有限公司 Reaction for preparing battery anode material precursor and purification system and process thereof

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KR20160077388A (en) * 2014-12-22 2016-07-04 주식회사 포스코 Precursor preparation reactor used for lithium battery materials
CN106745100A (en) * 2016-12-23 2017-05-31 荆门市格林美新材料有限公司 The preparation system and preparation method of battery-level lithium carbonate
CN206980732U (en) * 2017-07-28 2018-02-09 荆门市格林美新材料有限公司 A kind of Fast back-projection algorithm device of ternary anode material of lithium battery presoma

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KR19990015233A (en) * 1997-08-04 1999-03-05 손욱 Method for manufacturing double structure nickel hydroxide active material
CN103301794A (en) * 2013-05-20 2013-09-18 江苏凯力克钴业股份有限公司 Reaction process concentration control method of precursor for lithium battery material
CN203602368U (en) * 2013-10-28 2014-05-21 浙江东瓯过滤机制造有限公司 Spherical nickel hydroxide continuous synthesis device
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