CN108336314A - A kind of ternary precursor high-precision synthesis control method - Google Patents
A kind of ternary precursor high-precision synthesis control method Download PDFInfo
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- CN108336314A CN108336314A CN201711299266.0A CN201711299266A CN108336314A CN 108336314 A CN108336314 A CN 108336314A CN 201711299266 A CN201711299266 A CN 201711299266A CN 108336314 A CN108336314 A CN 108336314A
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- feeding groove
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- pid
- reaction kettle
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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
- H01M4/362—Composites
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
-
- 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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- 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
Abstract
The invention discloses a kind of ternary precursor high-precision synthesis control methods.Existing synthesis control mode control accuracy is low, and liquid inventory fluctuation is larger, and pH value is difficult to control, and overheating problem easily occurs in temperature in the kettle, and the stability that any of the above factor is all easily aligned into reaction impacts.The method of the present invention includes the constant flux control of ternary material NCM solution and ammonium hydroxide, the method for the constant flux control is as follows：Ternary material NCM solution and ammonium hydroxide are stored respectively in the feeding groove with permanent liquid level, reaction kettle is delivered to by the respective pump that feeds intake, there is the feeding groove of permanent liquid level to ensure the constant liquid level of feeding groove, the inlet liquid pressure remained steady for the pump that makes to feed intake.The present invention has effectively achieved the purpose that high-precision synthesizes control, improves the stability of synthetic reaction.
Description
Technical field
The present invention relates to ternary precursor synthesis technical field, especially a kind of ternary precursor high-precision synthesis controlling party
Method.
Background technology
Electric vehicle is commercially available quick development in recent years, thus brings the quick increasing of the power battery market demand
It is long.Nickel-cobalt-manganese ternary material lithium battery because with specific capacity height, good cycle, have a safety feature, it is cheap, be readily synthesized
The advantages that, it solves power battery performance and the balance of capacity well, has substantially met whole needs of power battery material,
It is acknowledged as one of most promising cobalt acid lithium alternative materials.
Building-up process is that a most important ring, the precision for synthesizing control determine product in ternary precursor material generating process
Quality and production stability, synthesis control accuracy it is higher, product quality is higher, production stabilization can also production cost be made to obtain
Effectively reduce.Common synthetic reaction controls liquid inventory by delivery pump combination regulating valve and enters reaction kettle；Pass through offline people
Work timing detection pH value and the mode for changing liquid caustic soda flow carry out control ph；Temperature in the kettle is controlled anti-by steam and regulating valve
Answer temperature in the kettle.This synthesis control mode, manual steps are more, and working strength is high, mistake easily occurs；Synthesis is from being fed to
Stability of flow needs a period of time, the unstable of start-up phase that can be synthetically produced certain influence, and this synthesis to subsequent
Control mode control accuracy is low, and liquid inventory fluctuation is larger, and pH value is difficult to control, and overheating problem easily occurs in temperature in the kettle,
The stability that any of the above factor is all easily aligned into reaction impacts.
Invention content
In view of the above technical problems, the present invention provides a kind of ternary precursor high-precision synthesis control method, passes through tool
The feeding groove control NCM solution and ammonium hydroxide of persevering liquid level are into kettle flow, the inlet liquid pressure remained steady for the pump that makes to feed intake, to have
Effect reduces influence of the transmission process pipeline crushing to discharge stability.
For achieving the above object, the present invention adopts the following technical scheme that：A kind of ternary precursor high-precision synthesis control
Method processed comprising the method for the constant flux control of ternary material NCM solution and ammonium hydroxide, the constant flux control is as follows：
Ternary material NCM solution and ammonium hydroxide are stored respectively in the feeding groove with permanent liquid level, it is defeated by the respective pump that feeds intake
It send to reaction kettle, there is the feeding groove of permanent liquid level to ensure the constant liquid level of feeding groove, the inlet liquid pressure for the pump that makes to feed intake is kept
Stablize.
As the supplement of above-mentioned technical proposal, the side wall upper part of the feeding groove is provided with overflow port, when molten in feeding groove
When liquid is higher than overflow port, corresponding holding tank is overflowed back by the overflow port, ensures the constant liquid level in feeding groove.
It is described that there is the feeding groove of permanent liquid level single pid loop to be combined to carry out flow control as the supplement of above-mentioned technical proposal
System, control NCM solution and ammonium hydroxide into kettle flow.
As the supplement of above-mentioned technical proposal, the pump that feeds intake is variable frequency pump, and the variable frequency pump is defeated by solution in feeding groove
It send to reaction kettle, by PID control, the flow signal of flowmeter detection inputs to PID, leads to the flowmeter of variable frequency pump and metering
It crosses compared with setting value, the signal of correction of deviation is exported to variable frequency pump, to eliminate flow error, reach the mesh of stability of flow
's.
As the supplement of above-mentioned technical proposal, solution, which enters, is equipped with triple valve on the pipeline of reaction kettle, pass through triple valve control
Solution processed enters reaction kettle or reflux；
When reaction kettle starts to feed intake, triple valve is first maintained at reflux direction, by the ratio, integral and the differential that adjust PID
Parameter makes solution actual flow automatic stabilisation within ± 0.5% deviation of setting value（Refer to when feeding intake can there are one it is theoretical into
Stream amount requires to be 100L/h such as feed rate, then practical feed rate can control between 99.5L/h-100.5L/h
Inlet amount is set to stablize）；Switching three-way valve to reaction kettle direction ensures that NCM and ammonium hydroxide are added when synthesis starts after stability of flow
The Stability and veracity of flow.
Further, the invention also includes the permanent pH of liquid caustic soda controls, and perseverance pH controls are cas PID control, and method is such as
Under：
Level-one PID detects pH value in kettle by pH transmitters and pH meter, and compared with setting pH value, will correct pH value deviation signal
As the setting value of two_stage flow PID, compared with the actual flow of liquid caustic soda, the signal for correcting flow deviation is exported to frequency conversion
Pump stablizes pH value to eliminate flow error by being automatically added to flux of alkaline liquor.
As the supplement of above-mentioned technical proposal, when reaction kettle starts to feed intake, liquid caustic soda triple valve is made to be maintained at reflux direction,
Two_stage flow PID control bound is consistent, so that lye is equivalent in constant flow mode operation, liquid caustic soda triple valve is mounted on
Liquid caustic soda enters on the pipeline of reaction kettle；After stability of flow, liquid caustic soda triple valve switches to reaction kettle direction, and by two_stage flow
The bound of PID control is set in OK range, so that the permanent pH of liquid caustic soda is controlled and is started.
As the supplement of above-mentioned technical proposal, the liquid caustic soda is also stored in the feeding groove with permanent liquid level, passes through throwing
Material pump is delivered to reaction kettle, and the side wall upper part of feeding groove is provided with overflow port, when the solution in feeding groove is higher than overflow port, passes through
The overflow port overflows back corresponding holding tank, ensures the constant liquid level in feeding groove.The present invention passes through feeding intake with permanent liquid level
Slot combination cascade PID carrys out control ph stabilization.
Further, the invention also includes thermostatic control in kettle, thermostatic control is mainly passed through by steam with condensed water pneumatic
Switch valve adjusts realization jointly, to achieve the purpose that temperature is stablized.
Further, the present invention is controlled by PLC control system, and each equipment operation is shown on Wincc control pictures
State and each generic operation.
The present invention has effectively achieved the purpose that high-precision synthesizes control, improves the stability of synthetic reaction；Automate journey
Degree is high, and avoid man-made failure operation factor influences caused by synthesis；It is high to synthesize control accuracy, technological parameter norm controlling is steady
Fixed, fluctuation is small；Synthesis control picture visual is strong, and historical record is checked conveniently.
Description of the drawings
Fig. 1 is the process flow chart in the embodiment of the present invention；
Fig. 2 is the constant flow in the embodiment of the present invention（NCM solution and ammonium hydroxide）PID control schematic diagram；
Fig. 3 is the permanent pH and constant flow in the embodiment of the present invention（Liquid caustic soda）PID control schematic diagram；
Fig. 4 is the thermostatic control schematic diagram in the embodiment of the present invention.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out specifically
It is bright.These embodiments are merely to illustrate the present invention, do not limit the scope of the invention in any way.Implementation based on the present invention
Example, various modifications, equivalent replacement and the improvement etc. that professional and technical personnel in the field make according to the present invention should all be included in this
Within the protection domain of invention.
Embodiment
NCM and ammonium hydroxide constant flux control
As shown in Figure 1, NCM, ammonia spirit are stored in holding tank, feeding intake with permanent liquid level is transported to by delivery pump respectively
In slot, a high position for the groove sidewall that feeds intake is provided with overflow port（Head tank is used i.e. in the present embodiment）, when in feeding groove solution higher than overflow
When head piece, holding tank is overflowed back by the overflow port, ensure that the constant liquid level in feeding groove, the inlet liquid pressure for the pump that makes to feed intake
Trying hard to keep, it is fixed to keep steady, and can effectively reduce influence of the pipeline crushing to discharge stability in transmission process.
The pump that feeds intake is variable frequency pump, which is delivered to reaction kettle by solution in feeding groove, and variable frequency pump is controlled with flowmeter by PID
Triple valve is first maintained at reflux direction by system in booting, by adjusting ratio, integral and the differential parameter of PID, keeps solution real
Border flow automatic stabilisation is within the scope of the certain positive and negative deviation of setting value（Flowed fluctuation can reach setting value in actual production process
Within deviation ± 0.5%）.Switching three-way valve is to reaction kettle direction after stability of flow, ensure that be added when synthesis starts NCM and
The Stability and veracity of ammonium hydroxide flow, PID control principle are illustrated in fig. 2 shown below.
Permanent pH controls
As shown in Figure 1, to be delivered to reaction kettle mode identical as NCM and ammonium hydroxide mode for liquid caustic soda.Synthesis is detected by pH meter in kettle
Solution ph, actual pH are exported the result for eliminating error to two_stage flow by level-one PID control compared with setting pH value
PID, as the setting value of two_stage flow PID, liquid caustic soda flow monitoring actual flow value, actual flow value and level-one PID output valves
Compare and calculate and control by two_stage flow PID, the result for eliminating flow error is exported to the pump that feeds intake, the flow of liquid caustic soda is made to protect
It is fixed to keep steady, and has both achieved the purpose that pH stablized or reach liquid caustic soda stability of flow in this way.
In booting, so that liquid caustic soda triple valve is maintained at reflux direction, two_stage flow PID control bound is consistent,
Lye is set to be equivalent in constant flow mode operation, after stability of flow（The fluctuation of lye instantaneous flow can be steady in actual moving process
It is scheduled within deviation ± 0.5% of setting value）, triple valve switches to reaction kettle direction, and will two_stage flow PID control up and down
Limit is set in OK range, so that the permanent pH of liquid caustic soda is controlled and is started to act on, pH's is steady at the beginning of ensuring that synthesis in this way
Fixed and liquid caustic soda flow stabilization.Permanent pH cas PID controls principle is as shown in Figure 3.
Thermostatic control
As shown in Figure 1, reaction kettle be jacket type, by temperature in the kettle meter detect reaction kettle in solution actual temperature, by with
Set temperature value compares, to control the action of steam pneumatic operated valve and cold water pneumatic operated valve, to by steam and cold water addition come
It is common to adjust temperature in the kettle, so that reactor temperature is reached setting value and keep stable, temperature fluctuation can in actual moving process
Stablize within deviation ± 0.1 DEG C of set temperature value, thermostatic control principle is as shown in Figure 4.
The foregoing is merely present pre-ferred embodiments, the embodiment and protection domain being not intended to limit the invention,
Based on the embodiment of the present invention, various modifications, equivalent replacement and the improvement that professional and technical personnel in the field make according to the present invention
Deng should all be included within protection scope of the present invention.
Claims (10)
1. a kind of ternary precursor high-precision synthesis control method, which is characterized in that including ternary material NCM solution and ammonium hydroxide
The method of constant flux control, the constant flux control is as follows：
Ternary material NCM solution and ammonium hydroxide are stored respectively in the feeding groove with permanent liquid level, it is defeated by the respective pump that feeds intake
It send to reaction kettle, there is the feeding groove of permanent liquid level to ensure the constant liquid level of feeding groove, the inlet liquid pressure for the pump that makes to feed intake is kept
Stablize.
2. ternary precursor high-precision synthesis control method according to claim 1, which is characterized in that the feeding groove
Side wall upper part is provided with overflow port, and when the solution in feeding groove is higher than overflow port, corresponding storage is overflowed back by the overflow port
Slot ensures the constant liquid level in feeding groove.
3. ternary precursor high-precision synthesis control method according to claim 1, which is characterized in that described that there is permanent liquid
The feeding groove of position combines single pid loop to carry out flow control.
4. ternary precursor high-precision synthesis control method according to claim 1, which is characterized in that the pump that feeds intake
For variable frequency pump, which is delivered to reaction kettle by solution in feeding groove, and variable frequency pump and the flowmeter of metering are controlled by PID
The flow signal of system, flowmeter detection inputs to PID, by the way that compared with setting value, the signal of correction of deviation is exported to frequency conversion
Pump, to eliminate flow error.
5. ternary precursor high-precision synthesis control method according to claim 1, which is characterized in that solution enters reaction
Triple valve is housed, controlling solution by triple valve enters reaction kettle or reflux on the pipeline of kettle；
When reaction kettle starts to feed intake, triple valve is first maintained at reflux direction, by the ratio, integral and the differential that adjust PID
Parameter makes solution actual flow automatic stabilisation within ± 0.5% deviation of setting value；Switching three-way valve is extremely after stability of flow
Reaction kettle direction ensures the Stability and veracity that NCM and ammonium hydroxide flow are added when synthesis starts.
6. ternary precursor high-precision synthesis control method according to claim 2, which is characterized in that further include liquid caustic soda
Permanent pH controls, perseverance pH controls are cas PID control, and method is as follows：
Level-one PID detects pH value in kettle by pH transmitters and pH meter, and compared with setting pH value, will correct pH value deviation signal
As the setting value of two_stage flow PID, compared with the actual flow of liquid caustic soda, the signal for correcting flow deviation is exported to frequency conversion
Pump stablizes pH value to eliminate flow error by being automatically added to flux of alkaline liquor.
7. ternary precursor high-precision synthesis control method according to claim 6, which is characterized in that
When reaction kettle starts to feed intake, so that liquid caustic soda triple valve is maintained at reflux direction, two_stage flow PID control bound is kept
Unanimously, lye is made to be equivalent in constant flow mode operation, liquid caustic soda triple valve enters mounted on liquid caustic soda on the pipeline of reaction kettle；It is flowing
After amount is stablized, liquid caustic soda triple valve switches to reaction kettle direction, and the bound of two_stage flow PID control is set in OK range
It is interior, so that the permanent pH of liquid caustic soda is controlled and starts.
8. ternary precursor high-precision synthesis control method according to claim 7, which is characterized in that the liquid caustic soda
It being stored in the feeding groove with permanent liquid level, reaction kettle is delivered to by the pump that feeds intake, the side wall upper part of feeding groove is provided with overflow port,
When the solution in feeding groove is higher than overflow port, corresponding holding tank is overflowed back by the overflow port, ensures the liquid in feeding groove
Position is constant.
9. ternary precursor high-precision synthesis control method according to claim 1, which is characterized in that further include permanent in kettle
Temperature control system, thermostatic control mainly adjust realization by pneumatic on-off valve jointly by steam and condensed water.
10. according to claim 1-9 any one of them ternary precursor high-precision synthesis control method, which is characterized in that logical
PLC control system control is crossed, and each equipment running status and each generic operation are shown on Wincc control pictures.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389328A (en) * | 2020-03-10 | 2020-07-10 | 湖南中伟新能源科技有限公司 | Automatic control method and system for preparing lithium ion battery anode material precursor |
| JP7353432B1 (en) | 2022-07-15 | 2023-09-29 | 住友化学株式会社 | Method for producing metal composite compound and lithium metal composite oxide |
| WO2024011625A1 (en) * | 2022-07-15 | 2024-01-18 | 宁德时代新能源科技股份有限公司 | Continuous reaction system, manganese iron oxalate precursor, lithium manganese iron phosphate, preparation method, and secondary battery |
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| CN111389328A (en) * | 2020-03-10 | 2020-07-10 | 湖南中伟新能源科技有限公司 | Automatic control method and system for preparing lithium ion battery anode material precursor |
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