CN111389328A - Automatic control method and system for preparing lithium ion battery anode material precursor - Google Patents

Automatic control method and system for preparing lithium ion battery anode material precursor Download PDF

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Publication number
CN111389328A
CN111389328A CN202010159683.0A CN202010159683A CN111389328A CN 111389328 A CN111389328 A CN 111389328A CN 202010159683 A CN202010159683 A CN 202010159683A CN 111389328 A CN111389328 A CN 111389328A
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China
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value
preset
reaction device
temperature
sending
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Inventor
徐祥
誾硕
王一乔
资旭晖
周明涛
周正
谢谊俊
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Hunan Zhongwei New Energy Technology Co ltd
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Hunan Zhongwei New Energy Technology 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
    • B01J19/0006—Controlling or regulating processes
    • 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
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • 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
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00177—Controlling or regulating processes controlling the pH
    • 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 an automatic control method and system for preparing a precursor of a lithium ion battery anode material. The control method comprises the following steps: sending an instruction to start a stirring motor in the reaction device; receiving the detected temperature in the reaction device, if the detected temperature of the reaction device reaches the preset temperature, sending an instruction to feed materials into the reaction device, and simultaneously sending an instruction to detect parameters in the reaction device; receiving a detection parameter value in the reaction device, comparing the detection parameter value of the reaction device with a preset parameter value, and if the detection parameter value of the reaction device is not consistent with the preset parameter value, sending an instruction to start a parameter adjusting system to adjust the parameter value until the detection value of the reaction device is consistent with the preset value; and after the preset reaction time is reached, sending an instruction to stop feeding into the reaction device, and after the interval time is reached, sending an instruction to close the stirring motor. The reaction is started and stopped, and the regulation and control of each process parameter in the reaction process are automated, so that the workload is reduced, the regulation and control are accurate, and the product has higher performance.

Description

Automatic control method and system for preparing lithium ion battery anode material precursor
Technical Field
The invention discloses a method and a system for automatically controlling the preparation reaction of a precursor of a lithium ion battery anode material.
Background
The lithium ion battery is a secondary battery, has the advantages of high energy density, high charge-discharge voltage, high energy density, long cycle life and the like, is widely applied to the aspects of small-sized electronic equipment, electric automobiles, spaceflight and the like, and is a representative of modern high-performance batteries.
The preparation method of the precursor of the lithium ion battery anode material mainly utilizes a wet chemical reaction, wherein factors such as reactant concentration, reaction temperature, stirring frequency and the like have important influence on the performance of the precursor, and the performance of the precursor has important influence on the performance of the lithium ion battery, so that the stability of each parameter in the precursor preparation reaction and the accuracy in parameter adjustment need to be strictly and accurately controlled in order to ensure the performance of the lithium ion battery.
At present, in the preparation reaction of the precursor of the positive electrode material of the lithium ion battery, the adjustment of various parameters and the detection and monitoring method of process data adopt artificial detection and adjustment, and the obtained precursor product has poor performance stability and large quality fluctuation and can not meet the requirement of the lithium ion battery on the performance of the precursor of the positive electrode material.
Disclosure of Invention
The invention provides an automatic control method for preparing a precursor of a lithium ion battery anode material, which is used for a central controller and comprises the following steps:
sending an instruction to start a stirring motor in the reaction device;
receiving the detected temperature in the reaction device, if the detected temperature of the reaction device reaches the preset temperature, sending an instruction to feed materials into the reaction device, and simultaneously sending an instruction to detect parameters in the reaction device;
receiving a detection parameter value in the reaction device, comparing the detection parameter value of the reaction device with a preset parameter value, and if the detection parameter value of the reaction device is not consistent with the preset parameter value, sending an instruction to start a parameter adjusting system to adjust the parameter value until the detection value of the reaction device is consistent with the preset value;
and after the preset reaction time is reached, sending an instruction to stop feeding into the reaction device, and after the interval time is reached, sending an instruction to close the stirring motor.
Preferably, the receiving a detection parameter value in the reaction device, comparing the detection parameter value of the reaction device with a preset parameter value, and if the detection parameter value of the reaction device is not consistent with the preset parameter value, sending an instruction to start the parameter adjusting system to adjust the parameter value until the detection value of the reaction device is consistent with the preset value includes:
receiving the detection temperature in the reaction device, comparing the detection temperature of the reaction device with the preset temperature, and if the detection temperature is not consistent with the preset temperature, sending an instruction to start a temperature adjusting system to adjust the temperature until the detection temperature of the reaction device is consistent with the preset temperature;
receiving a detected pH value in the reaction device, comparing the detected pH value with a preset pH value, and if the detected pH value is not consistent with the preset pH value, sending an instruction to start a pH value adjusting system to adjust the pH value until the detected pH value is consistent with the preset pH value;
and receiving a detected ammonia concentration value in the reaction device, comparing the detected ammonia concentration value with a preset ammonia concentration value, and if the detected ammonia concentration value is not consistent with the preset ammonia concentration value, sending an instruction to start an ammonia concentration value adjusting system to adjust the ammonia concentration value until the detected ammonia concentration value is consistent with the preset ammonia concentration value.
Preferably, the sending of the instruction starts the temperature adjusting system to adjust the temperature until the detected temperature of the reaction device is consistent with the preset temperature, and the method includes:
if the detection temperature of the reaction device is lower than the preset temperature, sending an instruction to communicate the heating device and the reaction device in the temperature regulating system, introducing hot water in the heating device into an outer jacket of the reaction device, and disconnecting the heating device and the reaction device when the detection temperature of the reaction device is increased to the preset temperature;
if the detected temperature of the reaction device is higher than the preset temperature, sending an instruction to communicate the cooling device and the reaction device in the temperature regulating system, introducing cold water in the cooling device into an outer jacket of the reaction device, and disconnecting the cooling device and the reaction device when the detected temperature of the reaction device is reduced to the preset temperature.
Preferably, the method further comprises the following steps:
receiving the detection temperature of the heating device, comparing the detection temperature of the heating device with a preset temperature, and if the detection temperature of the heating device is lower than the preset temperature, sending an instruction to open a steam inlet valve to enable steam to enter a steam heating pipe of the heating device to heat hot water of the heating device;
and receiving the detection temperature of the cooling device, comparing the detection temperature of the cooling device with a preset temperature, and if the detection temperature of the cooling device is higher than the preset temperature, sending an instruction to start the cooler to cool the cold water of the heating device.
Preferably, the sending instruction communicates the heating device and the reaction device in the temperature regulation system, and further includes:
sending an instruction to communicate an outlet of an outer layer jacket of the reaction device with a hot water reflux port of the heating device, and introducing water flowing out of the outlet of the outer layer jacket into the heating device;
the sending instruction communicates the cooling device and the reaction device in the temperature regulation system, and the method further comprises the following steps:
sending a command to communicate an outlet of an outer layer jacket of the reaction device with a cold water return port of a cooling device, and introducing water flowing out of the outlet of the outer layer jacket into the cooling device.
Preferably, the sending of the instruction to start the pH value adjusting system to adjust the pH value until the detected pH value is consistent with the preset pH value includes:
if the detected pH value is lower than the preset pH value, sending an instruction to increase the opening degree of a solenoid valve arranged on a connecting pipeline between a precipitator storage tank and the reaction device, and increasing the flow of the precipitator until the detected pH value is equal to the preset pH value;
if the detected pH value is higher than the preset pH value, an instruction is sent to reduce the opening degree of a solenoid valve arranged on a connecting pipeline between the precipitator storage tank and the reaction device, and the flow of the precipitator is reduced until the detected pH value is equal to the preset pH value.
Preferably, the sending an instruction to start the ammonia concentration value adjusting system to adjust the ammonia concentration value until the detected ammonia concentration value is consistent with the preset ammonia concentration value includes:
if the detected ammonia concentration value is lower than the preset ammonia concentration value, sending an instruction to increase the opening degree of a solenoid valve arranged on a connecting pipeline between a complexing agent ammonia water storage tank and the reaction device, and increasing the flow of the complexing agent ammonia water until the detected ammonia concentration value is equal to the preset ammonia concentration value;
if the detected ammonia concentration value is higher than the preset ammonia concentration value, sending an instruction to reduce the opening degree of a solenoid valve arranged on a connecting pipeline between the complexing agent ammonia water storage tank and the reaction device, and reducing the flow of the complexing agent ammonia water until the detected ammonia concentration value is equal to the preset ammonia concentration value.
Preferably, the control method further includes:
receiving the detection value of each solution flow at the inlet of the reaction device, and comparing the solution flow detection value with a preset value;
if the solution flow detection value is lower than the preset value, sending an instruction to increase the opening degree of an electromagnetic valve arranged on a connecting pipeline between the solution storage tank and the reaction device, and increasing the solution flow until the solution flow detection value is equal to the preset value;
and if the solution flow detection value is higher than the preset value, sending an instruction to reduce the opening degree of an electromagnetic valve arranged on a connecting pipeline between the solution storage tank and the reaction device, and reducing the solution flow until the solution flow detection value is equal to the preset value.
Preferably, the control method further includes:
monitoring the reaction time;
and determining preset parameter values according to the reaction time, wherein the preset parameter values comprise a preset temperature, a preset pH value, a preset ammonia concentration value and/or a preset solution flow value.
The invention also provides an automatic control system for preparing the lithium ion battery anode material precursor, which comprises a central controller, a reaction device, a temperature regulating system, a pH value regulating system and an ammonia concentration value regulating system;
the central controller comprises an upper computer and a P L C controller which are in signal connection, wherein the upper computer is used for setting preset values of various parameters, processing data and generating control instructions, and the P L C controller is used for receiving detection values of various parameters and sending the control instructions;
the reaction device is internally provided with a first temperature sensor, a pH sensor and an ammonia water concentration sensor which are respectively in signal connection with the P L C controller, and is also internally provided with a stirring device connected with a stirring motor, and the stirring motor is in signal connection with the P L C controller;
the temperature adjusting system comprises a heating device and a cooling device, wherein a second temperature sensor, a steam heating pipe, a hot water outlet and a hot water return port are arranged in the heating device, a high-temperature electromagnetic valve is arranged on a connecting pipeline of the steam heating pipe and a steam source, the hot water outlet is connected with an outer jacket inlet of the reaction device through a first connecting pipeline, a three-way electromagnetic valve is arranged on the first connecting pipeline, a hot water pump is arranged on a pipeline of the three-way electromagnetic valve and the hot water outlet, the hot water return port is connected with an outer jacket outlet of the reaction device, and a hot water return electromagnetic valve is arranged close to the hot water return port;
the pH value adjusting system comprises a precipitator storage tank, a first electromagnetic valve and a first electromagnetic flowmeter which are arranged on a connecting pipeline of the precipitator storage tank and the reaction device, and the first electromagnetic valve and the first electromagnetic flowmeter are in signal connection with the P L C controller;
the ammonia concentration value adjusting system comprises a complexing agent ammonia water storage tank, a second electromagnetic valve and a second electromagnetic flowmeter, wherein the second electromagnetic valve and the second electromagnetic flowmeter are arranged on a connecting pipeline of the complexing agent ammonia water storage tank and the reaction device, and the second electromagnetic valve and the second electromagnetic flowmeter are in signal connection with the P L C controller.
Drawings
FIG. 1 is a schematic structural diagram of an automatic control system for preparing a precursor of a lithium ion battery anode material according to the present invention;
fig. 2 is a schematic diagram of a connection structure between a P L C controller and other devices according to the present invention.
In the figure, the meaning of each symbol is as follows:
the device comprises a reaction device 10, a stirring motor 101, an ammonia water concentration sensor 102, a first temperature sensor 103, a pH sensor 104, a metal solution A storage tank 201, a metal solution B storage tank 202, a precipitant storage tank 203, a complexing agent ammonia water storage tank 204, a first electromagnetic valve 205, a second electromagnetic valve 206, a third electromagnetic valve 207, a fourth electromagnetic valve 208, a first electromagnetic flowmeter 209, a second electromagnetic flowmeter 210, a third electromagnetic flowmeter 211, a fourth electromagnetic flowmeter 212, a cooling device 30, a third temperature sensor 301, a cold water pump 302, a cooler 303, a cold water return electromagnetic valve 304, a heating device 40, a second temperature sensor 401, a high temperature electromagnetic valve 402, a steam heating pipe 403, a hot water pump 404, a hot water return electromagnetic valve 405, a three-way electromagnetic valve 50, a P L C controller 60 and an upper computer 70.
Detailed description of the preferred embodiments
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
The embodiment of the invention provides an automatic control method for preparing a precursor of a lithium ion battery anode material, which is used for a central controller, and the control method comprises the following steps:
sending an instruction to start a stirring motor in the reaction device;
receiving the detected temperature in the reaction device, if the detected temperature of the reaction device reaches the preset temperature, sending an instruction to feed materials into the reaction device, and simultaneously sending an instruction to detect parameters in the reaction device;
receiving a detection parameter value in the reaction device, comparing the detection parameter value of the reaction device with a preset parameter value, and if the detection parameter value of the reaction device is not consistent with the preset parameter value, sending an instruction to start a parameter adjusting system to adjust the parameter value until the detection value of the reaction device is consistent with the preset value;
and after the preset reaction time is reached, sending an instruction to stop feeding into the reaction device, and after the interval time is reached, sending an instruction to close the stirring motor.
By adopting the control method, the automatic control of the reaction process for preparing the lithium ion battery anode material precursor can be realized, wherein the reaction starting and stopping are included, the regulation and control of each process parameter in the reaction process can be realized automatically, the automation degree of the reaction control and the process parameter adjustment is high, the workload is reduced, meanwhile, the regulation and control of each process parameter are more accurate, the product granularity distribution is narrower, the performance is higher, the material waste caused by the regulation and control lag and the like is avoided, the solid content of the material in the reaction device is increased, and the efficiency is improved.
In one embodiment of the invention, the detected temperature in the reaction device is received, the detected temperature of the reaction device is compared with the preset temperature, and if the detected temperature of the reaction device is not consistent with the preset temperature, an instruction is sent to start the temperature regulating system to regulate the temperature until the detected temperature of the reaction device is consistent with the preset temperature;
receiving a detected pH value in the reaction device, comparing the detected pH value with a preset pH value, and if the detected pH value is not consistent with the preset pH value, sending an instruction to start a pH value adjusting system to adjust the pH value until the detected pH value is consistent with the preset pH value;
and receiving a detected ammonia concentration value in the reaction device, comparing the detected ammonia concentration value with a preset ammonia concentration value, and if the detected ammonia concentration value is not consistent with the preset ammonia concentration value, sending an instruction to start an ammonia concentration value adjusting system to adjust the ammonia concentration value until the detected ammonia concentration value is consistent with the preset ammonia concentration value.
The method provided by the invention can realize the detection and regulation of the temperature, the pH value and the ammonia concentration value in the reaction device, so that the detection values of all parameters can be basically consistent with the preset values, and the theoretical requirements of the reaction process on the process parameter values are basically met.
Because the temperature, the pH value and the ammonia concentration value have important influence on the performance of the precursor of the lithium ion battery anode material, the method mainly detects and regulates the three parameters, so that the detection values of the three parameters can be basically consistent with preset values, the theoretical requirements of the reaction process on the process parameter values are basically met, the precursor obtained by the reaction has higher performance, and the requirement of the lithium ion battery anode material on high performance is met.
As can be appreciated by those skilled in the art, other process parameters in the reaction process can also be detected and controlled.
If the detected temperature of the reaction device is lower than the preset temperature, sending an instruction to communicate the heating device and the reaction device in the temperature regulating system, introducing hot water in the heating device into an outer jacket of the reaction device, and disconnecting the heating device and the reaction device when the detected temperature of the reaction device is increased to the preset temperature;
if the detected temperature of the reaction device is higher than the preset temperature, sending an instruction to communicate the cooling device and the reaction device in the temperature regulating system, introducing cold water in the cooling device into an outer jacket of the reaction device, and disconnecting the cooling device and the reaction device when the detected temperature of the reaction device is reduced to the preset temperature.
By adopting the method, the automatic control of the temperature in the reaction device can be realized.
In the actual use process, a connecting pipeline can be arranged between the heating device and the outer jacket of the reaction device, a connecting pipeline is arranged between the cooling device and the outer jacket of the reaction device, an electromagnetic valve is arranged on the pipeline, a controller sends an instruction to the electromagnetic valve, the opening of the electromagnetic valve is adjusted or the electromagnetic valve is controlled to be opened or closed, and therefore the automatic regulation and control of the temperature in the reaction device are achieved.
In addition, a water pump can be arranged on the connecting pipeline, hot water in the heating device or cold water in the cooling device is pumped into an outer jacket of the reaction device, and the controller sends an instruction to the water pump to control the water pump to be turned on or off, so that the flow of the hot water or the cold water is realized.
The automatic control method provided by the invention further comprises the following steps:
receiving the detection temperature of the heating device, comparing the detection temperature of the heating device with a preset temperature, and if the detection temperature of the heating device is lower than the preset temperature, sending an instruction to open a steam inlet valve to enable steam to enter a steam heating pipe of the heating device to heat hot water of the heating device;
and receiving the detection temperature of the cooling device, comparing the detection temperature of the cooling device with a preset temperature, and if the detection temperature of the cooling device is higher than the preset temperature, sending an instruction to start the cooler to cool the cold water of the heating device.
The method can automatically control the temperature of the hot water in the heating device, so that the temperature of the hot water in the heating device can be kept within a preset range, and the reaction requirement can be met when the hot water is used for heating the reaction device.
Meanwhile, the method can automatically control the temperature of the cold water in the cooling device, so that the temperature of the cold water can be kept within a preset range, and the requirement of reaction can be met when the cold water is used for cooling the reaction device. In the actual use process, the controller can send an instruction to the cooler, and the cooler is started to cool the cold water. Thereby realizing the automatic control of the temperature of the cold water in the cooling device.
In a preferred embodiment of the present invention, the sending instruction communicates the heating device and the reaction device in the temperature adjustment system, further comprising:
sending an instruction to communicate an outlet of an outer layer jacket of the reaction device with a hot water reflux port of the heating device, and introducing water flowing out of the outlet of the outer layer jacket into the heating device;
the sending instruction communicates the cooling device and the reaction device in the temperature regulation system, and the method further comprises the following steps:
sending a command to communicate an outlet of an outer layer jacket of the reaction device with a cold water return port of a cooling device, and introducing water flowing out of the outlet of the outer layer jacket into the cooling device.
By adopting the method, the hot water and the cold water in the heating device and the cooling device can be respectively recovered, so that the hot water and the cold water can be recycled, and the resources are saved.
In the actual use process, electromagnetic valves can be respectively arranged on a communication pipeline between an outlet of an outer layer jacket of the reaction device and a hot water return port of the heating device and a communication pipeline between an outlet of the outer layer jacket of the reaction device and a cold water return port of the cooling device, and the hot water or cold water in the outer layer jacket can automatically return by sending an opening and closing instruction to the electromagnetic valves through the controller.
Specifically, when controlling the hot water reflux, the electromagnetic valve arranged on the communication pipeline between the outlet of the outer jacket of the reaction device and the cold water reflux port of the cooling device needs to be closed, and the electromagnetic valve arranged on the communication pipeline between the outlet of the outer jacket of the reaction device and the hot water reflux port of the heating device needs to be opened; when cold water reflux is controlled, an electromagnetic valve arranged on a communication pipeline between an outlet of an outer layer jacket of the reaction device and a cold water reflux port of the cooling device needs to be opened, and an electromagnetic valve arranged on a communication pipeline between the outlet of the outer layer jacket of the reaction device and a hot water reflux port of the heating device needs to be closed.
In one embodiment of the invention, if the detected pH value is lower than the preset pH value, an instruction is sent to increase the opening degree of a solenoid valve arranged on a connecting pipeline between the precipitator storage tank and the reaction device, and the flow of the precipitator is increased until the detected pH value is equal to the preset pH value;
if the detected pH value is higher than the preset pH value, an instruction is sent to reduce the opening degree of a solenoid valve arranged on a connecting pipeline between the precipitator storage tank and the reaction device, and the flow of the precipitator is reduced until the detected pH value is equal to the preset pH value.
By adopting the method, the automatic control of the pH value in the reaction device can be realized, so that the pH value in the reaction device can be kept in a preset range.
In the actual use process, a connecting pipeline can be arranged between the precipitant storage tank and the reaction device, an electromagnetic valve is arranged on the pipeline, a controller sends an instruction to the electromagnetic valve, and the opening of the electromagnetic valve is adjusted or the electromagnetic valve is controlled to be opened or closed, so that the automatic regulation and control of the pH value in the reaction device are realized.
In another embodiment of the invention, if the detected ammonia concentration value is lower than the preset ammonia concentration value, an instruction is sent to increase the opening degree of a solenoid valve arranged on a connecting pipeline between the complexing agent ammonia water storage tank and the reaction device, and the flow of the complexing agent ammonia water is increased until the detected ammonia concentration value is equal to the preset ammonia concentration value;
if the detected ammonia concentration value is higher than the preset ammonia concentration value, sending an instruction to reduce the opening degree of a solenoid valve arranged on a connecting pipeline between the complexing agent ammonia water storage tank and the reaction device, and reducing the flow of the complexing agent ammonia water until the detected ammonia concentration value is equal to the preset ammonia concentration value.
By adopting the method, the automatic control of the ammonia concentration value in the reaction device can be realized, so that the ammonia concentration value in the reaction device can be kept in a preset range.
In the actual use process, a connecting pipeline can be arranged between the complexing agent ammonia water storage tank and the reaction device, an electromagnetic valve is arranged on the pipeline, a controller sends an instruction to the electromagnetic valve, the opening degree of the electromagnetic valve is adjusted or the electromagnetic valve is controlled to be opened or closed, and therefore the automatic regulation and control of the ammonia concentration value in the reaction device are achieved.
The control method provided by the embodiment of the invention further comprises the following steps:
receiving the detection value of each solution flow at the inlet of the reaction device, and comparing the solution flow detection value with a preset value;
if the solution flow detection value is lower than the preset value, sending an instruction to increase the opening degree of an electromagnetic valve arranged on a connecting pipeline between the solution storage tank and the reaction device, and increasing the solution flow until the solution flow detection value is equal to the preset value;
and if the solution flow detection value is higher than the preset value, sending an instruction to reduce the opening degree of an electromagnetic valve arranged on a connecting pipeline between the solution storage tank and the reaction device, and reducing the solution flow until the solution flow detection value is equal to the preset value.
By adopting the method, the automatic control of the feeding amount can be realized, so that the flow of each material entering the reaction device can be kept within a preset range.
In the actual use process, a connecting pipeline can be arranged between the material storage tank and the reaction device, an electromagnetic valve is arranged on the pipeline, the controller sends an instruction to the electromagnetic valve, the opening degree of the electromagnetic valve is adjusted or the electromagnetic valve is controlled to be opened or closed, and therefore the material flow can be automatically regulated and controlled.
The method for automatically controlling the preparation reaction of the lithium ion battery anode material precursor provided by the embodiment of the invention also comprises the following steps:
monitoring the reaction time;
and determining preset parameter values according to the reaction time, wherein the preset parameter values comprise a preset temperature, a preset pH value, a preset ammonia concentration value and/or a preset solution flow value.
By adopting the method, automatic control of different parameter values in different reaction times can be realized.
In practical application, the parameter values of different reaction times can be preset, for example, in the first reaction time, the preset temperature is T1, in the second reaction time, the preset temperature is T2, in the regulation and control process, the controller can automatically monitor the reaction time, if in the first reaction time, the regulated and controlled detection temperature is equal to the preset temperature T1, and if in the second reaction time, the regulated and controlled detection temperature is equal to the preset temperature T2. Thereby realizing the regulation and control of the reaction temperature in different reaction time.
In the same way, the regulation and control of the pH value, the ammonia concentration value and the solution flow value in different reaction time can be realized.
FIG. 1 and FIG. 2 show an implementation environment of a control method provided by an embodiment of the present invention, wherein FIG. 1 provides a structure of an automatic control system for preparing a precursor of a lithium ion battery cathode material, FIG. 2 provides a connection structure of a P L C controller and other devices, in FIG. 2, temperature sensors comprise all temperature sensors in the control system, solenoid valves comprise all solenoid valves in the control system, water pumps comprise all water pumps in the control system, and solenoid valve flow meters comprise all solenoid valve flow meters in the control system, the control system comprises a central controller, a reaction device 10, a temperature regulation system, a pH value regulation system and an ammonia concentration value regulation system;
the central controller comprises an upper computer 70 and a P L C controller 60 which are in signal connection, wherein the upper computer 70 is used for setting preset values of various parameters, processing data and generating control instructions, and the P L C controller 60 is used for receiving detection values of various parameters and sending the control instructions;
a first temperature sensor 103, a pH sensor 104 and an ammonia water concentration sensor 102 which are respectively in signal connection with the P L C controller 60 are arranged in the reaction device 10, a stirring device connected with a stirring motor 101 is also arranged in the reaction device 10, and the stirring motor 101 is in signal connection with the P L C controller 60;
the temperature adjusting system comprises a heating device 40 and a cooling device 30, wherein a second temperature sensor 401, a steam heating pipe 403, a hot water outlet and a hot water return port are arranged in the heating device 40, a high-temperature electromagnetic valve 402 is arranged on a connecting pipeline of the steam heating pipe 403 and a steam source, the hot water outlet is connected with an outer jacket inlet of the reaction device 10 through a first connecting pipeline, a three-way electromagnetic valve 50 is arranged on the first connecting pipeline, a hot water pump 404 is arranged on a pipeline of the three-way electromagnetic valve 50 and the hot water outlet, the hot water return port is connected with the outer jacket outlet of the reaction device 10, a hot water return electromagnetic valve 405 is arranged close to the hot water return port, a third temperature sensor 301, a cooler 303, a cold water outlet and a cold water return port are arranged in the cooling device 30, the cold water outlet is connected with the outer jacket inlet of the reaction device 10 through a second connecting pipeline, the three-way electromagnetic valve 50 is arranged on the second connecting pipeline, a pipeline of the three-way electromagnetic valve 50 and the cold water outlet is provided with a cold water pump 302, the cold water return electromagnetic valve 304, a cold water return signal electromagnetic valve 304, a cold water pump 304, a cold water return electromagnetic valve 304, a cold water return signal controller 401, a cold water return port, a cold water return solenoid valve 401, a cold;
the pH value adjusting system comprises a precipitator storage tank 203, a third electromagnetic valve 207 and a third electromagnetic flowmeter 211 which are arranged on a connecting pipeline of the precipitator storage tank 203 and the reaction device 10, and the third electromagnetic valve 207 and the third electromagnetic flowmeter 211 are in signal connection with the P L C controller 60;
the ammonia concentration value adjusting system comprises a complexing agent ammonia water storage tank 204, a fourth electromagnetic valve 208 and a fourth electromagnetic flowmeter 212 which are arranged on a connecting pipeline of the complexing agent ammonia water storage tank 204 and the reaction device 10, wherein the fourth electromagnetic valve 208 and the fourth electromagnetic flowmeter 212 are in signal connection with the P L C controller 60.
The method for automatically controlling the reaction by using the reaction system can comprise the following steps:
before starting the reaction, inputting various reaction parameters including temperature, various solution flow rates, a pH control range, a complexing agent concentration, a stirring motor frequency and the like into an upper computer 70, in the initial stage of the reaction, outputting a signal to a stirring motor 101 by a P L C controller 60, detecting the temperature in a reaction device by a first temperature sensor, sending the detected temperature to a P L C controller, comparing the detected temperature with a preset temperature in the upper computer, starting the reaction when the detected temperature of the reaction device reaches the preset value, sending a signal to an electromagnetic valve 205 and 208 by the P L C controller according to various process parameter values preset in the upper computer, opening the electromagnetic valve bank, feeding back a signal to a P L C controller by an electromagnetic flow meter group 209 and 212, sending a signal to adjust the valve size of the electromagnetic valve bank 205 and 208 when the solution flow rate exceeds the control range, achieving the purpose of controlling the solution flow rate by the P L C controller, and sending a signal to a P L C controller to control equipment L to control the P3660 according to the input process parameters and control the change of the P3660.
The pH sensor 104 feeds back a pH signal in the reaction device to the P L C controller 60, when the pH is smaller than the control range, the P L C controller 60 sends a signal to the third electromagnetic valve 207 to increase the opening degree of the third electromagnetic valve 207 so as to increase the flow rate of the precipitant to increase the pH in the reaction device, and when the pH value fed back by the pH sensor 104 is larger than a set value, the P L C controller 60 sends a signal to the second electromagnetic valve 207 to decrease the opening degree of the third electromagnetic valve 207 so as to decrease the flow rate of the precipitant to decrease the pH in the reaction device.
The ammonia concentration sensor 102 feeds back an ammonia concentration signal to the P L C controller 60, when the ammonia concentration is lower than a set value, the P L C controller 60 sends a signal to the fourth electromagnetic valve 208 to increase the opening degree of the fourth electromagnetic valve 208 and increase the flow rate of the complexing agent ammonia water to improve the ammonia concentration in the reaction, and when the ammonia concentration sensor 102 feeds back the ammonia water concentration higher than the set value, the P L C controller 60 sends a signal to the fourth electromagnetic valve 208 to decrease the opening degree of the fourth electromagnetic valve 208 to reduce the flow rate of the complexing agent ammonia water to reduce the ammonia water concentration in the reaction.
When the temperature fed back by the temperature sensor 103 is higher than the set value, the P L C controller 60 sends a signal to the three-way solenoid valve 50 to heat the reaction device 10, when the temperature in the reaction device reaches the set value, the three-way solenoid valve 50 and the hot water return solenoid valve 405 are closed, the hot water pump 404 stops working, the hot water return solenoid valve 304 and the cold water return solenoid valve 304 are closed, the hot water pump 404 starts working, the hot water in the heating device 40 is pumped into the outer jacket of the reaction device 10 to heat the reaction device 10, when the temperature in the reaction device reaches the set value, the three-way solenoid valve 50 and the hot water return solenoid valve 405 are closed, the hot water pump 404 stops working, when the temperature fed back by the temperature sensor 103 is higher than the set value, the P L C controller 60 sends a signal to the three-way solenoid valve 50, the valve is opened to the cooling device 40 side, the hot water return solenoid valve 405 is closed, the cold water return solenoid valve 304 is opened, the cold water pump 302 starts working, the cold water return solenoid valve 302 pumps the reaction device 10 into the outer jacket of the reaction device to stop working, and the cold water return solenoid valve 304 and the reaction device stops working.
When the temperature fed back by the second temperature sensor 401 of the heating apparatus is lower than the temperature set value, the P L C controller 60 sends a signal to the high temperature solenoid valve 402, the high temperature solenoid valve is opened, the steam enters the steam heating pipe 403, the temperature in the heating apparatus rises, and when the temperature reaches the set value, the high temperature solenoid valve 402 is closed.
When the temperature fed back from the third temperature sensor 301 of the cooling device is lower than the temperature set point, the P L C controller 60 sends a signal to the cooler 303, the cooler 303 starts to operate, the cooling device temperature decreases, and when the temperature reaches the set point, the cooler 303 stops operating.
After the reaction time is up, the upper computer 70 sends a signal to the P L C controller 60, the P L C controller 60 sends a signal, the electromagnetic valve bank 205 and 208 are closed, the reaction is stopped, the stirring motor 101 is closed after the reaction time is up, and the precursor is discharged to perform the next process.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention. It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (10)

1. An automatic control method for preparing a precursor of a lithium ion battery cathode material is characterized by being used for a central controller, and comprises the following steps:
sending an instruction to start a stirring motor in the reaction device;
receiving the detected temperature in the reaction device, if the detected temperature of the reaction device reaches the preset temperature, sending an instruction to feed materials into the reaction device, and simultaneously sending an instruction to detect parameters in the reaction device;
receiving a detection parameter value in the reaction device, comparing the detection parameter value of the reaction device with a preset parameter value, if the detection parameter value is not consistent with the preset parameter value, sending an instruction to start a parameter adjusting system, and adjusting the parameter value until the detection value of the reaction device is consistent with the preset value;
and after the preset reaction time is reached, sending an instruction to stop feeding into the reaction device, and after the interval time is reached, sending an instruction to close the stirring motor.
2. The automatic control method for preparing a precursor of a lithium ion battery cathode material of claim 1, wherein the step of receiving a detection parameter value in the reaction device, comparing the detection parameter value with a preset parameter value, and if the detection parameter value is not consistent with the preset parameter value, sending an instruction to start the parameter adjusting system to adjust the parameter value until the detection value of the reaction device is consistent with the preset value comprises the steps of:
receiving the detection temperature in the reaction device, comparing the detection temperature of the reaction device with the preset temperature, if the detection temperature is not consistent with the preset temperature, sending an instruction to start a temperature adjusting system, and adjusting the temperature until the detection temperature of the reaction device is consistent with the preset temperature;
receiving a detected pH value in the reaction device, comparing the detected pH value with a preset pH value, if the detected pH value is not consistent with the preset pH value, sending an instruction to start a pH value adjusting system, and adjusting the pH value until the detected pH value is consistent with the preset pH value;
and receiving a detected ammonia concentration value in the reaction device, comparing the detected ammonia concentration value with a preset ammonia concentration value, and if the detected ammonia concentration value is inconsistent with the preset ammonia concentration value, sending an instruction to start an ammonia concentration value adjusting system, and adjusting the ammonia concentration value until the detected ammonia concentration value is consistent with the preset ammonia concentration value.
3. The automatic control method for preparing the precursor of the lithium ion battery cathode material according to claim 2, wherein the sending of the instruction starts a temperature adjusting system, and the adjusting of the temperature until the detected temperature of the reaction device is consistent with a preset temperature comprises:
if the detection temperature of the reaction device is lower than the preset temperature, sending an instruction to communicate the heating device and the reaction device in the temperature regulating system, introducing hot water in the heating device into an outer jacket of the reaction device, and disconnecting the heating device and the reaction device when the detection temperature of the reaction device is increased to the preset temperature;
if the detected temperature of the reaction device is higher than the preset temperature, sending an instruction to communicate the cooling device and the reaction device in the temperature regulating system, introducing cold water in the cooling device into an outer jacket of the reaction device, and disconnecting the cooling device and the reaction device when the detected temperature of the reaction device is reduced to the preset temperature.
4. The automatic control method for preparing a precursor of a positive electrode material of a lithium ion battery according to claim 3, further comprising:
receiving the detection temperature of the heating device, comparing the detection temperature of the heating device with a preset temperature, and if the detection temperature of the heating device is lower than the preset temperature, sending an instruction to open a steam inlet valve to enable steam to enter a steam heating pipe of the heating device to heat hot water of the heating device;
and receiving the detection temperature of the cooling device, comparing the detection temperature of the cooling device with a preset temperature, and if the detection temperature of the cooling device is higher than the preset temperature, sending an instruction to start the cooler to cool the cold water of the heating device.
5. The automatic control method for preparing a precursor of a positive electrode material of a lithium ion battery according to claim 3,
the sending instruction communicates heating device and reaction unit in the temperature regulation system, still includes:
sending an instruction to communicate an outlet of an outer layer jacket of the reaction device with a hot water reflux port of the heating device, and introducing water flowing out of the outlet of the outer layer jacket into the heating device;
the sending instruction communicates the cooling device and the reaction device in the temperature regulation system, and the method further comprises the following steps:
sending a command to communicate an outlet of an outer layer jacket of the reaction device with a cold water return port of a cooling device, and introducing water flowing out of the outlet of the outer layer jacket into the cooling device.
6. The automatic control method for preparing a precursor of a positive electrode material of a lithium ion battery according to claim 2, wherein the sending of the command starts a pH adjusting system to adjust the pH value until the detected pH value is consistent with a preset pH value, and the method comprises the following steps:
if the detected pH value is lower than the preset pH value, sending an instruction to increase the opening degree of a solenoid valve arranged on a connecting pipeline between a precipitator storage tank and the reaction device, and increasing the flow of the precipitator until the detected pH value is equal to the preset pH value;
if the detected pH value is higher than the preset pH value, an instruction is sent to reduce the opening degree of a solenoid valve arranged on a connecting pipeline between the precipitator storage tank and the reaction device, and the flow of the precipitator is reduced until the detected pH value is equal to the preset pH value.
7. The automatic control method for preparing a precursor of a lithium ion battery anode material according to claim 2, wherein the sending of the instruction starts an ammonia concentration value adjusting system, and the adjusting of the ammonia concentration value until the detected ammonia concentration value is consistent with a preset ammonia concentration value comprises:
if the detected ammonia concentration value is lower than the preset ammonia concentration value, sending an instruction to increase the opening degree of a solenoid valve arranged on a connecting pipeline between a complexing agent ammonia water storage tank and the reaction device, and increasing the flow of the complexing agent ammonia water until the detected ammonia concentration value is equal to the preset ammonia concentration value;
if the detected ammonia concentration value is higher than the preset ammonia concentration value, sending an instruction to reduce the opening degree of a solenoid valve arranged on a connecting pipeline between the complexing agent ammonia water storage tank and the reaction device, and reducing the flow of the complexing agent ammonia water until the detected ammonia concentration value is equal to the preset ammonia concentration value.
8. The automatic control method for preparing a precursor of a positive electrode material of a lithium ion battery according to claim 2, wherein the control method further comprises:
receiving the detection value of each solution flow at the inlet of the reaction device, and comparing the solution flow detection value with a preset value;
if the solution flow detection value is lower than the preset value, sending an instruction to increase the opening degree of an electromagnetic valve arranged on a connecting pipeline between the solution storage tank and the reaction device, and increasing the solution flow until the solution flow detection value is equal to the preset value;
and if the solution flow detection value is higher than the preset value, sending an instruction to reduce the opening degree of an electromagnetic valve arranged on a connecting pipeline between the solution storage tank and the reaction device, and reducing the solution flow until the solution flow detection value is equal to the preset value.
9. The automatic control method for preparing a precursor of a positive electrode material of a lithium ion battery according to claim 2, wherein the control method further comprises:
monitoring the reaction time;
and determining preset parameter values according to the reaction time, wherein the preset parameter values comprise a preset temperature, a preset pH value, a preset ammonia concentration value and/or a preset solution flow value.
10. An automatic control system for preparing a precursor of a lithium ion battery anode material is characterized by comprising a central controller, a reaction device, a temperature regulating system, a pH value regulating system and an ammonia concentration value regulating system;
the central controller comprises an upper computer and a P L C controller which are in signal connection, wherein the upper computer is used for setting preset values of various parameters, processing data and generating control instructions, and the P L C controller is used for receiving detection values of various parameters and sending the control instructions;
the reaction device is internally provided with a first temperature sensor, a pH sensor and an ammonia water concentration sensor which are respectively in signal connection with the P L C controller, and is also internally provided with a stirring device connected with a stirring motor, and the stirring motor is in signal connection with the P L C controller;
the temperature adjusting system comprises a heating device and a cooling device, wherein a second temperature sensor, a steam heating pipe, a hot water outlet and a hot water return port are arranged in the heating device, a high-temperature electromagnetic valve is arranged on a connecting pipeline of the steam heating pipe and a steam source, the hot water outlet is connected with an outer jacket inlet of the reaction device through a first connecting pipeline, a three-way electromagnetic valve is arranged on the first connecting pipeline, a hot water pump is arranged on a pipeline of the three-way electromagnetic valve and the hot water outlet, the hot water return port is connected with an outer jacket outlet of the reaction device, and a hot water return electromagnetic valve is arranged close to the hot water return port;
the pH value adjusting system comprises a precipitator storage tank, a first electromagnetic valve and a first electromagnetic flowmeter which are arranged on a connecting pipeline of the precipitator storage tank and the reaction device, and the first electromagnetic valve and the first electromagnetic flowmeter are in signal connection with the P L C controller;
the ammonia concentration value adjusting system comprises a complexing agent ammonia water storage tank, a second electromagnetic valve and a second electromagnetic flowmeter, wherein the second electromagnetic valve and the second electromagnetic flowmeter are arranged on a connecting pipeline of the complexing agent ammonia water storage tank and the reaction device, and the second electromagnetic valve and the second electromagnetic flowmeter are in signal connection with the P L C controller.
CN202010159683.0A 2020-03-10 2020-03-10 Automatic control method and system for preparing lithium ion battery anode material precursor Pending CN111389328A (en)

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KR20160077388A (en) * 2014-12-22 2016-07-04 주식회사 포스코 Precursor preparation reactor used for lithium battery materials
CN108336314A (en) * 2017-12-08 2018-07-27 华友新能源科技（衢州）有限公司 A kind of ternary precursor high-precision synthesis control method
CN110098393A (en) * 2019-04-23 2019-08-06 金川集团股份有限公司 A kind of method that three stage controls method prepares narrow size distribution nickel cobalt aluminium positive electrode material precursor
CN110294498A (en) * 2018-03-24 2019-10-01 圣戈莱（北京）科技有限公司 A kind of intelligent control reaction system preparing ternary material precursor and preparation method

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Publication number Priority date Publication date Assignee Title
KR20160077388A (en) * 2014-12-22 2016-07-04 주식회사 포스코 Precursor preparation reactor used for lithium battery materials
CN204720500U (en) * 2015-04-30 2015-10-21 浙江天能能源科技有限公司 Produce the device of polynary positive pole material of lithium ion cell presoma
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