Electrolysis device and method for reducing nonmetal impurities of rare earth

Abstract

The invention relates to the technical field of data processing, and discloses an electrolysis device and method for reducing nonmetal impurities in rare earth, and the device comprises an electrolysis module, a compensation signal generation module, a regenerative electrolyte system acquisition module, an impedance correction parameter generation module and a pulse impurity removal module. The anode gas and the cathode sediment of the electrolyzed rare earth are obtained; according to the component proportion of the anode gas, a compensation signal for secondary electrolysis of the rare earth is generated; adding a compensating agent into the molten electrolyte according to the compensation signal to generate a regenerated electrolyte system of the rare earth; generating an impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system; pulse current is applied to the rare earth based on the impedance correction parameters, and impurity-removed rare earth is obtained; the rare earth impurity removal effect can be improved.

Description

Technical Field

[0001] The present invention relates to the technical field of data processing, and in particular to a rare earth electrolysis device and method for reducing non-metallic impurities. Background Art

[0002] During the rare earth electrolysis production process, existing technologies are ineffective at removing non-metallic impurities, making it difficult to control impurity levels at low levels. This results in insufficient purity in the resulting rare earth products, making them unable to meet the demands of high-precision applications. Furthermore, due to inaccurate control of the reaction process during the impurity removal process, impurity removal is often incomplete or new impurities are introduced during the removal process, seriously impacting the performance and stability of the rare earth products.

[0003] At the same time, existing electrolysis systems have poor adaptability, with electrolyte composition easily becoming unbalanced as the reaction proceeds. This lacks an effective regulatory mechanism to maintain its optimal state, resulting in low electrolysis efficiency and significant fluctuations in impurity removal effectiveness. Furthermore, current parameters are often set in a fixed mode, unable to dynamically adjust to real-time changes in interface conditions during the electrolysis process. This further restricts the efficient removal of non-metallic impurities and makes it difficult to achieve the desired results of rare earth electrolysis impurity removal. Summary of the Invention

[0004] The present invention provides a rare earth electrolysis device and method for reducing non-metallic impurities, the main purpose of which is to solve the problem of poor rare earth electrolysis effect.

[0005] To achieve the above-mentioned object, the present invention provides an electrolysis device for reducing non-metallic impurities in rare earth, characterized in that the device includes an electrolysis module, a compensation signal generation module, a regeneration electrolyte system acquisition module, an impedance correction parameter generation module and a pulse impurity removal module, wherein: The electrolysis module is used to apply an initial current density to the electrolytic cell to perform electrolysis, thereby obtaining anode gas and cathode deposits of rare earths after electrolysis; The compensation signal generating module is used to generate a compensation signal for secondary electrolysis of the rare earth according to the component ratio of the anode gas; The regenerative electrolyte system acquisition module is used to add a compensating agent to the molten electrolyte according to the compensation signal to generate the regenerative electrolyte system of the rare earth; The impedance correction parameter generating module is used to generate the impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system; The pulse de-doping module is used to apply a pulse current to the rare earth based on the impedance correction parameter to obtain the de-doped rare earth.

[0006] In a preferred embodiment, the initial current density includes: Generate a baseline value based on the initial conductivity of the electrolyte; The reference value is matched with a preset current density comparison table to obtain the initial current density of the electrolytic cell.

[0007] In a preferred embodiment, when the compensation signal generating module generates the compensation signal for the secondary electrolysis of the rare earth according to the component ratio of the anode gas, it is specifically used to: detecting a volume ratio of hydrogen fluoride to carbon dioxide in the anode gas; When the volume ratio exceeds a preset threshold, a compensation signal for the electrolytic cell is generated.

[0008] In a preferred embodiment, when the regenerative electrolyte system acquisition module adds a compensating agent to the molten electrolyte according to the compensation signal to generate the rare earth regenerative electrolyte system, it is specifically used to: adding an alkali metal carbonate to the molten electrolyte according to a compensator type in the compensation signal; The electrolysis temperature is maintained within a preset time, and the rare earth carbonate precipitate is removed by filtration to obtain a regenerated electrolyte system of the rare earth.

[0009] In a preferred embodiment, when the impedance correction parameter generation module generates the impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system, it is specifically used to: Applying a sinusoidal current between the cathode deposit of the electrolytic cell and the regeneration electrolyte system to generate an electrode interface response signal of the rare earth; The voltage and current phase differences and amplitude ratios of the electrode interface response signals at different frequencies are collected as cathode interface impedance spectrum data of the rare earth; Fitting an equivalent circuit model to the rare earth based on the cathode interface impedance spectrum data to obtain a resistance value of the rare earth; According to the change rate of the resistance value and the initial resistance value, a preset impedance correction coefficient mapping table is matched to obtain the impedance correction coefficient of the rare earth.

[0010] In a preferred embodiment, when performing equivalent circuit model fitting on the rare earth based on the cathode interface impedance spectrum data to obtain the resistance value of the rare earth, the impedance correction parameter generation module is specifically used to: Construct a three-element equivalent circuit model; Inputting the cathode interface impedance spectrum data into the three-element equivalent circuit model and performing linear fitting; The fitting parameter value of the charge transfer resistance element in the three-element equivalent circuit model after linear fitting is extracted as the resistance value of the rare earth.

[0011] In a preferred embodiment, the impedance correction parameter generation module is specifically used to: Obtaining a baseline resistance value during the initial electrolysis stage; determining a rate of change of the resistance value according to a ratio of the resistance value to the reference resistance value; The change rate is input into a preset impedance correction coefficient mapping table, and an impedance correction coefficient linearly corresponding to the change rate is output.

[0012] In a preferred embodiment, when the pulse impurity removal module applies a pulse current to the rare earth based on the impedance correction parameter to obtain the impurity-removed rare earth, it is specifically used to: Dynamically adjusting the peak current density of the pulse current according to the impedance correction parameter; applying a pulse sequence to the cathode of the electrolytic cell with the adjusted sell power parameters; After completing the preset pulse cycle, the impurity-removed rare earth is obtained.

[0013] In a preferred embodiment, when the pulse impurity removal module dynamically adjusts the peak current density of the pulse current according to the impedance correction parameter, the calculation formula of the peak current density is as follows:

[0014] Where, is the peak current density, is the cathode reaction activation factor, is the mass of cathode deposit, is the impedance correction factor, is the duration of a single pulse; The output current is dynamically adjusted according to the peak current density.

[0015] In order to solve the above problems, the present invention also provides a rare earth electrolysis method for reducing non-metallic impurities, the method comprising: S1. Applying an initial current density to the electrolytic cell to perform electrolysis, thereby obtaining anode gas and cathode deposits of rare earths after electrolysis; S2. generating a compensation signal for secondary electrolysis of the rare earth according to the component ratio of the anode gas; S3, adding a compensating agent to the molten electrolyte according to the compensation signal to generate a regenerated electrolyte system of the rare earth; S4, generating an impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system; S5. Applying a pulse current to the rare earth based on the impedance correction parameter to obtain the impurity-removed rare earth.

[0016] Compared with the prior art, the present invention has the following beneficial effects: 1. This invention significantly improves rare earth impurity removal through the synergistic effect of multiple modules. The electrolysis module, combined with the scientific setting of the initial current density, lays a good foundation for subsequent impurity removal. The compensation signal generation module accurately generates compensation signals based on the proportion of anode gas components. The regenerative electrolyte system acquisition module optimizes the electrolyte composition accordingly, ensuring a stable and efficient electrolysis environment, fundamentally enhancing the targetedness and effectiveness of impurity removal.

[0017] 2. The present invention uses an impedance correction parameter generation module to generate correction parameters based on the cathode interface impedance. The pulse impurity removal module dynamically adjusts the pulse current accordingly, achieving precise control of the impurity removal process. This dynamic adaptation approach can fully cope with the complex changes in the electrolysis process, significantly improving the removal efficiency of non-metallic impurities, ultimately obtaining a rare earth product with higher purity and better performance, effectively enhancing the overall effectiveness of rare earth electrolysis impurity removal. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 A system architecture diagram of a rare earth electrolysis device for reducing non-metallic impurities provided by one embodiment of the present invention; Figure 2 A schematic flow chart of a rare earth electrolysis method for reducing non-metallic impurities provided in one embodiment of the present invention.

[0019] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION

[0020] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments belong to some embodiments of the present invention, but not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts shall fall within the scope of protection of the present invention.

[0021] The terms used in the embodiments of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The singular forms "said" and "the" used in the embodiments of the present invention and the appended claims are also intended to include plural forms, unless the context clearly indicates otherwise, and "a plurality" generally includes at least two.

[0022] As used herein, the words “if” or “when” may be interpreted as “at the time of” or “when” or “in response to determining” or “in response to detecting,” depending on the context. Similarly, the phrases “if it is determined” or “if (stated condition or event) is detected” may be interpreted as “when it is determined” or “in response to the determination” or “when detecting (stated condition or event)” or “in response to detecting (stated condition or event),” depending on the context.

[0023] In addition, the step sequence in the following method embodiments is only an example and not a strict limitation.

[0024] In practice, the server-side device deployed for the rare earth electrolysis device for reducing non-metallic impurities may consist of one or more devices. The rare earth electrolysis device for reducing non-metallic impurities can be implemented as a service instance, a virtual machine, or a hardware device. For example, the rare earth electrolysis device for reducing non-metallic impurities can be implemented as a service instance deployed on one or more devices in a cloud node. Simply put, the rare earth electrolysis device for reducing non-metallic impurities can be understood as software deployed on a cloud node, providing the rare earth electrolysis device for reducing non-metallic impurities to each client. Alternatively, the rare earth electrolysis device for reducing non-metallic impurities can be implemented as a virtual machine deployed on one or more devices in a cloud node. This virtual machine contains application software for managing each client. Alternatively, the rare earth electrolysis device for reducing non-metallic impurities can be implemented as a server-side device composed of multiple hardware devices of the same or different types, with one or more hardware devices configured to provide the rare earth electrolysis device for reducing non-metallic impurities to each client.

[0025] In terms of implementation, the rare earth electrolysis device for reducing non-metallic impurities and the user end are mutually compatible. Specifically, if the rare earth electrolysis device for reducing non-metallic impurities is an application installed on a cloud service platform, the user end is the client that establishes a communication connection with the application; or if the rare earth electrolysis device for reducing non-metallic impurities is implemented as a website, the user end is implemented as a webpage; or if the rare earth electrolysis device for reducing non-metallic impurities is implemented as a cloud service platform, the user end is implemented as a mini-program within an instant messaging application.

[0026] like Figure 1 1 is a system architecture diagram of a rare earth electrolysis device for reducing non-metallic impurities provided by one embodiment of the present invention.

[0027] The rare earth electrolysis device for reducing non-metallic impurities 100 described in the present invention can be installed in a cloud server. In terms of implementation, it can be implemented as one or more service devices, as an application installed in the cloud (e.g., a mobile service operator's server, server cluster, etc.), or developed as a website. Depending on the functionality implemented, the rare earth electrolysis device for reducing non-metallic impurities 100 can include an electrolysis module 101, a compensation signal generation module 102, a regenerative electrolyte system acquisition module 103, an impedance correction parameter generation module 104, and a pulse impurity removal module 105. A module, also referred to as a unit, is a series of computer program segments that can be executed by an electronic device processor and perform a fixed function. These modules are stored in the electronic device's memory.

[0028] In an embodiment of the present invention, in the rare earth electrolysis device for reducing non-metallic impurities, each of the above modules can be implemented independently and called with other modules. The call here can be understood as that a certain module can connect to multiple modules of another type and provide corresponding services to the multiple modules connected to it. In the rare earth electrolysis device for reducing non-metallic impurities provided by an embodiment of the present invention, the scope of application of the rare earth electrolysis device for reducing non-metallic impurities can be adjusted by adding modules and directly calling them without modifying the program code, thereby realizing cluster-type horizontal expansion, so as to achieve the purpose of quickly and flexibly expanding the rare earth electrolysis device for reducing non-metallic impurities. In actual applications, the above modules can be set in the same device or different devices, or they can be set in a virtual device, such as a service instance in a cloud server.

[0029] The following describes the various components and specific workflow of the rare earth electrolysis device for reducing non-metallic impurities in conjunction with specific embodiments: The electrolysis module 101 is used to apply an initial current density to the electrolytic cell to perform electrolysis, thereby obtaining anode gas and cathode sediment of rare earth after electrolysis; In an embodiment of the present invention, the initial current density includes: Generate a baseline value based on the initial conductivity of the electrolyte; The reference value is matched with a preset current density comparison table to obtain the initial current density of the electrolytic cell.

[0030] Specifically, use a conductivity meter to measure the initial conductivity of the electrolyte. Before measurement, check whether the probe of the conductivity meter is clean. If there is any stain, rinse it with deionized water and wipe it dry. Then immerse the probe completely in the electrolyte, making sure that the probe does not contact the container wall. At the same time, place the container containing the electrolyte in a constant temperature device, adjust the constant temperature device to stabilize the electrolyte temperature within the preset operating temperature range, and continuously observe the temperature display. After the temperature has not fluctuated for 5 consecutive minutes, start the conductivity meter and observe the displayed value of the meter. When the value remains unchanged for 30 consecutive seconds, press the record button of the meter and determine the value recorded at this time as the baseline value.

[0031] Furthermore, the preset current density comparison table is formed in a laboratory environment. First, a variety of electrolyte samples with different conductivities are selected, and the conductivities of these samples cover all ranges that may appear in actual production. Then, each sample is placed in an electrolytic cell with the same specifications as in actual production, and an electrolysis test is carried out under the same environmental conditions. During the test, the optimal current density of the electrolytic cell corresponding to each sample is recorded, and then the conductivity of each sample is used as a benchmark value and arranged one by one with the corresponding optimal current density to form a preset current density comparison table. Each row in the table clearly marks a benchmark value and the corresponding electrolytic cell current density. Then, the generated benchmark value is compared one by one with the benchmark value in the comparison table. Starting from the first row of the table, check whether the benchmark value of each row is the same as the generated benchmark value. When exactly the same benchmark value is found, extract the current density corresponding to the row. This current density is the initial current density of the electrolytic cell.

[0032] In general, by applying an initial current density determined based on the initial conductivity of the electrolyte for electrolysis, stable initial reaction conditions can be provided for the entire impurity removal process, ensuring the orderly start of the electrolysis process. At the same time, the anode gas and cathode deposits after electrolysis can be accurately obtained, providing reliable basic data for the work of subsequent modules and ensuring the targetedness and effectiveness of subsequent impurity removal steps.

[0033] The compensation signal generating module 102 is configured to generate a compensation signal for secondary electrolysis of the rare earth according to the component ratio of the anode gas; In an embodiment of the present invention, when the compensation signal generating module generates the compensation signal for the secondary electrolysis of the rare earth according to the component ratio of the anode gas, it is specifically configured to: detecting a volume ratio of hydrogen fluoride to carbon dioxide in the anode gas; When the volume ratio exceeds a preset threshold, a compensation signal for the electrolytic cell is generated.

[0034] Specifically, a gas sampling device is used to collect gas samples from the anode area of the electrolytic cell. Before sampling, it is necessary to check whether the connecting parts of the sampling device are tight. The sealing can be judged by applying soapy water on the interface to observe whether bubbles are generated to ensure that there is no leakage. The air inlet of the sampling device is connected to the anode gas outlet through a special polytetrafluoroethylene pipe with a smooth inner wall. The length of the pipe is controlled within 1 meter to reduce gas retention. The valve is opened to allow the gas to continue to flow into the sampling device at a flow rate of 2 liters per second for 5 minutes. During this period, the flow meter in the device is observed to ensure that the flow rate is stable to discharge the residual air in the device. Then the valve is closed, and the sampling device is slowly removed and passed through a special Use the interface to connect to the inlet of the gas chromatograph, start the gas chromatograph, set the column temperature to 60°C, use nitrogen as the carrier gas and control the flow rate at 30 ml per minute, use a thermal conductivity detector as the detector, let the gas sample enter the chromatographic column through the injection valve, hydrogen fluoride and carbon dioxide will gradually separate due to their different adsorption and desorption abilities in the chromatographic column, after the separation is completed, the thermal conductivity detector will output corresponding electrical signals according to the difference in thermal conductivity of the two gases, the instrument display will convert these electrical signals into the volume ratio of hydrogen fluoride and carbon dioxide in the gas sample, use the instrument's built-in printing function to print out and record these two volume ratio values.

[0035] Furthermore, the preset threshold is that before the electrolyzer leaves the factory, it undergoes a 100-hour continuous normal operation test, records the volume ratio of hydrogen fluoride to carbon dioxide in the anode gas at different time periods, takes the maximum safe value as the preset threshold and stores it in the memory of the electrolyzer control system, and inputs the detected volume ratio of hydrogen fluoride to carbon dioxide into the control system. The system will automatically call the preset threshold in the memory, compare the two values, and determine whether the detected volume ratio exceeds the preset threshold. If it exceeds the preset threshold, the control system will immediately send a trigger instruction to the signal generation module. After receiving the instruction, the module generates an electrical signal lasting 10 seconds according to the voltage range and pulse frequency that can be recognized by the electrolyzer adjustment actuator. This electrical signal is the compensation signal of the electrolyzer. After generation, it is directly transmitted to the adjustment actuator of the electrolyzer through a shielded cable. After receiving the signal, the actuator begins to adjust the operating parameters of the electrolyzer.

[0036] In general, generating a compensation signal for secondary electrolysis based on the component ratio of the anode gas can respond to changes in gas composition during the electrolysis process in real time, and promptly capture the imbalance tendency of the electrolysis system through signal feedback, providing an accurate basis for subsequent adjustment of the electrolyte composition, thereby enhancing the dynamic control capability of the electrolysis reaction process.

[0037] The regenerative electrolyte system acquisition module 103 is configured to add a compensating agent to the molten electrolyte according to the compensation signal to generate the rare earth regenerative electrolyte system; In an embodiment of the present invention, when the regeneration electrolyte system acquisition module adds a compensating agent to the molten electrolyte according to the compensation signal to generate the rare earth regeneration electrolyte system, it is specifically used to: adding an alkali metal carbonate to the molten electrolyte according to a compensator type in the compensation signal; The electrolysis temperature is maintained within a preset time, and the rare earth carbonate precipitate is removed by filtration to obtain a regenerated electrolyte system of the rare earth.

[0038] Specifically, after receiving the compensation signal from the electrolytic cell, the signal is transmitted to a dedicated analysis device, which analyzes the type of compensator by identifying the specific frequency band in the signal. Different types of compensators correspond to different frequency bands, such as sodium carbonate corresponds to the 100 Hz frequency band and potassium carbonate corresponds to the 200 Hz frequency band. After the analysis is completed, the device display will clearly show the type of alkali metal carbonate that needs to be added. According to the display results, the corresponding alkali metal carbonate solid with a purity of 99.9% is selected and placed in a ceramic grinding device with a smooth inner wall. The grinding head of the grinding device rotates at a speed of 300 revolutions per minute and continues to grind for 20 minutes to make the solid into particles. The powder is uniform in weight and free of lumps, and then transferred to the weighing pan of an electronic scale with an accuracy of 0.01 g. When weighing, ensure that there is no airflow interference around. Record the mass after the displayed value stabilizes. Pour the weighed powder carefully into the feeding funnel with a polytetrafluoroethylene valve. The funnel outlet is facing the center of the molten electrolyte in the electrolytic cell. Open the valve and control the powder falling speed to 0.5 g per second by adjusting the valve opening and closing. During the feeding process, use a high-temperature resistant glass stirring rod to gently stir the molten electrolyte to ensure that the powder is evenly dispersed. After the feeding is completed, close the valve and continue stirring for 5 minutes to fully mix the alkali metal carbonate and the molten electrolyte.

[0039] Furthermore, after the addition of alkali metal carbonate and stirring are completed, the temperature control system of the electrolytic cell is immediately started. The temperature sensor of the system is a platinum resistance sensor, which is inserted into the molten electrolyte at a depth of 10 cm. It monitors the temperature in real time and transmits the data to the control module. The preset electrolysis temperature value has been stored in the control module in advance. When the monitored temperature is 1°C lower than the preset value, the control module triggers the electric heating device to start. The heating power of the heating device is 5 kilowatts. When the monitored temperature reaches the preset value, the control module issues an instruction to stop the heating device. This cycle keeps the electrolysis temperature stable within a preset time (such as 2 hours). After the preset time, the control module automatically cuts off the power supply of the heating device and allows the molten electrolyte to cool naturally. The temperature is recorded every 30 minutes during the cooling process. When the temperature drops to 25°C (room temperature), it is ready for filtration. The filter funnel is cloth The funnel is 20 cm in diameter. The filter cloth in the funnel is a polytetrafluoroethylene filter cloth with a pore size of 0.22 μm. The edge of the filter cloth extends 2 cm beyond the edge of the funnel and is fixed. The bottom of the funnel is connected to a clean glass container with a volume of 5 liters through a rubber stopper. The cooled molten electrolyte is slowly poured into the funnel. The pouring speed is controlled at 100 ml per minute to avoid liquid overflow. The liquid is allowed to flow through the filter cloth into the container below due to gravity. The filter cloth will intercept all rare earth carbonate precipitates. After all the liquid is filtered, the precipitate in the funnel is rinsed twice with 50 ml of deionized water, and the rinsing liquid is also collected in the container. The transparent liquid collected in the container at this time is the regenerated electrolyte system of the rare earth. The rare earth carbonate precipitate on the filter cloth is carefully removed with tweezers, placed in a dry porcelain crucible, and dried in a 60°C oven for 2 hours. After removal, it is stored in a sealed polyethylene bottle.

[0040] In general, adding compensators to the molten electrolyte according to the compensation signal and generating a regenerated electrolyte system can effectively optimize the composition and state of the electrolyte, maintain the stability and activity of the electrolyte system, avoid the decrease in impurity removal efficiency due to electrolyte imbalance, and create a suitable reaction environment for subsequent impedance detection and pulse impurity removal.

[0041] The impedance correction parameter generating module 104 is used to generate the impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system; In an embodiment of the present invention, when the impedance correction parameter generation module generates the impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system, it is specifically used to: Applying a sinusoidal current between the cathode deposit of the electrolytic cell and the regeneration electrolyte system to generate an electrode interface response signal of the rare earth; The voltage and current phase differences and amplitude ratios of the electrode interface response signals at different frequencies are collected as cathode interface impedance spectrum data of the rare earth; Fitting an equivalent circuit model to the rare earth based on the cathode interface impedance spectrum data to obtain a resistance value of the rare earth; According to the change rate of the resistance value and the initial resistance value, a preset impedance correction coefficient mapping table is matched to obtain the impedance correction coefficient of the rare earth.

[0042] When performing equivalent circuit model fitting on the rare earth based on the cathode interface impedance spectrum data to obtain the resistance value of the rare earth, the impedance correction parameter generation module is specifically used to: Construct a three-element equivalent circuit model; Inputting the cathode interface impedance spectrum data into the three-element equivalent circuit model and performing linear fitting; The fitting parameter value of the charge transfer resistance element in the three-element equivalent circuit model after linear fitting is extracted as the resistance value of the rare earth.

[0043] When the impedance correction parameter generation module performs matching of a preset impedance correction coefficient mapping table according to the change rate of the resistance value and the initial resistance value to obtain the impedance correction coefficient of the rare earth, it is specifically used to: Obtaining a baseline resistance value during the initial electrolysis stage; determining a rate of change of the resistance value according to a ratio of the resistance value to the reference resistance value; The change rate is input into a preset impedance correction coefficient mapping table, and an impedance correction coefficient linearly corresponding to the change rate is output.

[0044] Specifically, an AC signal is applied to the electrode interface at multiple different frequencies. After the signal stabilizes at each frequency, the voltage and current phase difference and amplitude ratio of the electrode interface response signal are recorded. These phase differences and amplitude ratios recorded at all frequencies are organized in order, and the resulting data set is the cathode interface impedance spectrum data of the rare earth.

[0045] Furthermore, open the preset equivalent circuit model software, which stores the equivalent circuit model designed for the rare earth electrolysis system, and import the cathode interface impedance spectrum data of the rare earth into the software. The software will automatically call the built-in fitting function, and adjust the parameters of each component in the model so that the impedance spectrum calculated by the model coincides with the imported cathode interface impedance spectrum data. When the two completely coincide, the software will display the corresponding value of the resistance element in the model, which is the resistance value of the rare earth.

[0046] Furthermore, the rate of change of the resistance value of the rare earth and the initial resistance value is calculated. The initial resistance value is the resistance data measured and stored when the rare earth does not participate in the electrolysis reaction. The rate of change is the ratio of the difference between the current resistance value and the initial resistance value to the initial resistance value. The preset impedance correction coefficient mapping table is established in the laboratory through a large number of experiments. Each row in the table contains a change rate and a corresponding impedance correction coefficient. The calculated change rate is compared one by one with the change rate in the mapping table. After finding a completely consistent entry, the value corresponding to the entry is extracted. This value is the impedance correction coefficient of the rare earth.

[0047] Specifically, the three-element equivalent circuit model consists of a solution resistance element connected in series, a charge transfer resistance element connected in parallel, and an electric double layer capacitance element. The solution resistance element uses a standard resistor with an accuracy of 0.1 ohm, which is specifically used to simulate the resistance characteristics generated when the molten electrolyte solution in the rare earth electrolysis system conducts current. The charge transfer resistance element uses an adjustable precision resistance module to accurately reflect the resistance formed during the electron transfer process at the electrode and electrolyte interface. The electric double layer capacitance element selects an electrolytic capacitor with a withstand voltage value that meets the requirements of the electrolysis system, which is used to characterize the capacitance properties of the double layer formed due to charge separation when the electrode surface contacts the electrolyte. The above three elements are retrieved through the component library of the circuit design software. The charge transfer resistance element and the electric double layer capacitance element are first connected in parallel to form a parallel unit, and then the parallel unit is connected in series with the solution resistance element to form a complete three-element equivalent circuit model. After the connection is completed, the connection relationship is checked by the verification function of the software. After confirmation, the model is saved in a special format to the model database of the equivalent circuit fitting software.

[0048] Further, open the fitting software that stores the three-element equivalent circuit model, click the "Data Import" button in the menu bar of the software main interface, a file selection window pops up, browse and select the cathode interface impedance spectrum data file of the rare earth that has been organized in the specified format in the window, which contains the voltage and current phase difference and amplitude ratio information at different frequencies, click the "Format Check" button at the bottom of the window, the software automatically checks whether the data arrangement, unit marking, etc. of the file are consistent with the software requirements, after the check is passed, click the "Confirm Import" button to complete the data import, find and click the name of the constructed three-element equivalent circuit model in the model selection bar on the left side of the software, and put it in Select the state, then click the "Linear Fit" function key in the toolbar. The software will immediately start the fitting program and compare the impedance value corresponding to each data point in the cathode interface impedance spectrum data with the theoretically calculated impedance value of the three-element equivalent circuit model under the same frequency conditions. The parameter values of the solution resistance element, charge transfer resistance element and double-layer capacitance element in the model are changed through the built-in adjustment mechanism, so that the impedance curve calculated by the model and the measured curve formed by the data points are gradually approached. Continue to adjust until the overlap of the two curves reaches the highest level and the deviation value between the curves is stable within the minimum range and no longer changes. At this time, the software automatically stops adjusting and completes the linear fitting process.

[0049] Furthermore, after the linear fitting is completed, the software automatically jumps to the result display interface. In the "Component Parameters" section of the interface, find the parameter column marked as "Charge Transfer Resistor Element". The value displayed in digital form in the parameter column is the fitting parameter value of the component determined after linear fitting. Use the "Value Extraction" tool of the software to click on the parameter column, extract the displayed value to the clipboard, and then paste it into the data recording table. This value is the resistance value of the rare earth. Click the "Data Save" button of the software to associate the resistance value with the corresponding cathode interface impedance spectrum data and the fitting curve image and store them in the designated folder of the data storage system. The folder is named "Rare Earth Resistance Value Record" so that it can be called when calculating the impedance correction coefficient later. Specifically, after the electrolytic cell is started and enters the initial electrolysis stage, that is, within the first hour after the start of the electrolysis reaction, the same implementation process of constructing a three-element equivalent circuit model and extracting the rare earth resistance value is followed, and the same electrochemical workstation, equivalent circuit fitting software and three-element equivalent circuit model are used to process the electrode interface response signal in the rare earth electrolysis system at this time, extract the fitting parameter value of the charge transfer resistance element, determine this value as the baseline resistance value of the initial electrolysis stage, and store it in a dedicated folder of the data storage system, and the folder is named "initial baseline data."

[0050] Furthermore, the previously recorded and saved resistance value of the rare earth is retrieved from the data storage system, and the stored reference resistance value is retrieved at the same time. The resistance value is compared with the reference resistance value, and the resistance value is divided by the reference resistance value. The result is the ratio of the resistance value to the reference resistance value. The ratio reflects the change of the resistance value relative to the reference resistance value. This ratio is the rate of change of the resistance value. The calculated rate of change is recorded in the data recording table and saved in association with the corresponding resistance value and reference resistance value information.

[0051] Furthermore, a preset impedance correction coefficient mapping table is pre-established in the data processing software. The table contains multiple sets of corresponding data of change rates and impedance correction coefficients, and these data show a linear correspondence. Open the data processing software, find the operation interface of the preset impedance correction coefficient mapping table, enter the determined rate of change of the resistance value in the input field, and the software will automatically search for the impedance correction coefficient that linearly corresponds to the change rate in the mapping table. After finding it, the impedance correction coefficient is displayed in the output field, and the output impedance correction coefficient is exported and saved in the result file for parameter adjustment of the subsequent electrolysis process.

[0052] In general, the impedance correction parameters generated based on the cathode interface impedance of the regenerated electrolyte system can accurately reflect the changes in the electrochemical state of the cathode interface. Through equivalent circuit model fitting and parameter calculation, the interface impedance is converted into a quantifiable correction basis, providing scientific parameter support for the dynamic adjustment of the pulse current and improving the accuracy of the impurity removal process.

[0053] The pulse de-doping module 105 is configured to apply a pulse current to the rare earth based on the impedance correction parameter to obtain de-doped rare earth.

[0054] In an embodiment of the present invention, when the pulse decontamination module applies a pulse current to the rare earth based on the impedance correction parameter to obtain the decontaminated rare earth, it is specifically configured to: Dynamically adjusting the peak current density of the pulse current according to the impedance correction parameter; applying a pulse sequence to the cathode of the electrolytic cell with the adjusted sell power parameters; After completing the preset pulse cycle, the impurity-removed rare earth is obtained.

[0055] When the pulse impurity removal module dynamically adjusts the peak current density of the pulse current according to the impedance correction parameter, the calculation formula of the peak current density is as follows:

[0056] Where, is the peak current density, is the cathode reaction activation factor, is the mass of cathode deposit, is the impedance correction factor, is the duration of a single pulse; The output current is dynamically adjusted according to the peak current density.

[0057] Specifically, the saved impedance correction coefficient is retrieved from the result file and input into the pulse current control system. The system has a preset correspondence between the impedance correction coefficient and the peak current density of the pulse current. After the impedance correction coefficient is input, the system will automatically adjust the internal current regulation module according to this correspondence, change the peak current density of the output pulse current, and make the peak current density match the input impedance correction coefficient. After the adjustment is completed, the system display will show the new peak current density value. After confirming that the value is stable, the parameter will be locked to ensure the stability of the subsequent pulse current output.

[0058] Furthermore, after the pulse current control system adjusts the peak current density, the operator checks whether the connection between the cathode of the electrolytic cell and the pulse current output end is firm. The connection point needs to be clamped with a special clamp to ensure that there is no looseness or poor contact. Then, the "Pulse Sequence Output" option is selected on the operation interface of the control system. The system will generate a pulse current and transmit it to the cathode of the electrolytic cell according to the preset pulse frequency, pulse width and other parameters, combined with the adjusted peak current density. The current continues to act on the electrolysis system through the cathode. During this process, the control system monitors the output status of the pulse current in real time. If an abnormality occurs, the output will be automatically stopped and an alarm will be issued. Under normal circumstances, the pulse sequence will continue to be applied to the cathode.

[0059] Furthermore, the preset pulse period refers to the action time of the pulse sequence required to complete a complete impurity removal. This time has been pre-set and stored in the control system. When the action time of the pulse sequence on the cathode reaches the preset pulse period, the control system will automatically cut off the pulse current output, and the operator will turn off the power of the electrolytic cell. After the temperature of the electrolysis system drops to room temperature, the cell cover of the electrolytic cell is opened, and a special corrosion-resistant spoon is used to remove the solid substance generated on the cathode surface. This substance is the rare earth after impurity removal. It is placed in a clean ceramic dish and rinsed three times with deionized water to remove the residual electrolyte on the surface. It is then placed in a drying oven and dried at 80°C for 2 hours to obtain dry rare earth after impurity removal.

[0060] Specifically, the cathode reaction activation factor is a fixed value obtained by arithmetically averaging the activation energy data of multiple parallel tests in a laboratory simulation system using the same rare earth electrolytic cell, molten electrolyte and cathode material as in actual production, and measuring the activation energy of the cathode reaction at different electrolysis stages. Once determined, this value is stored in the parameter library of the pulse current control system.

[0061] Furthermore, the quality of cathode deposits is monitored in real time by a high-precision piezoelectric sensor installed inside the cathode base during the process of pulse current acting on the cathode of the electrolytic cell. The sensor fits tightly against the cathode surface and can sense changes in deposit thickness and convert them into quality data, transmitting real-time values to the control system every 0.1 seconds.

[0062] Furthermore, the impedance correction coefficient comes from a preset impedance correction coefficient mapping table, which is established by applying different impedance conditions to the rare earth electrolysis system in the laboratory and recording the corresponding correction requirements. When the rate of change of the resistance value is input into the data processing software, the software will retrieve the value linearly corresponding to the change rate from the mapping table as the impedance correction coefficient.

[0063] Furthermore, the duration of a single pulse action is determined during the electrolytic cell debugging phase. By testing the influence of pulse currents at different durations on the impurity removal effect, the duration that can achieve the highest impurity removal efficiency is selected as a fixed value and stored in the program of the pulse current control system. It remains unchanged throughout the entire impurity removal process.

[0064] Furthermore, the significance of this formula lies in integrating the key factors that affect the peak value of the pulse current, reflecting the activity characteristics of the reaction itself through the cathode reaction activation factor, reflecting the current load situation of the cathode surface in combination with the real-time cathode deposit mass, and adjusting with the help of the impedance correction coefficient to adapt to the impedance changes of the electrolysis system. Then, based on the fixed single pulse action duration, the peak current density that can accurately match the current electrolysis state is jointly calculated to ensure that the pulse current can effectively promote impurity separation without causing excessive cathode reaction due to excessive current.

[0065] Furthermore, when the cathode reaction activation factor and the duration of a single pulse remain unchanged, if the cathode deposit mass increases and the impedance correction coefficient remains stable, the peak current density will increase with the increase in cathode deposit mass. If the impedance correction coefficient increases and the cathode deposit mass remains unchanged, the peak current density will increase with the increase in the impedance correction coefficient. When the cathode deposit mass decreases or the impedance correction coefficient decreases, the peak current density will decrease accordingly under the condition that other conditions remain unchanged. That is, the peak current density shows a synchronous increase and decrease relationship with the cathode deposit mass and the impedance correction coefficient.

[0066] In general, by applying pulse current to rare earths based on impedance correction parameters, parameters such as the peak density of the pulse current can be dynamically adjusted according to the real-time changes in the cathode interface state, so that the pulse impurity removal process is highly adapted to the actual state of the electrolysis system, thereby maximizing the removal efficiency of non-metallic impurities and ultimately obtaining rare earth products with higher purity, which directly improves the impurity removal effect.

[0067] Reference Figure 2FIG. 1 is a flow chart of a rare earth electrolysis method for reducing non-metallic impurities according to an embodiment of the present invention. In this embodiment, the rare earth electrolysis method for reducing non-metallic impurities includes: S1. Applying an initial current density to the electrolytic cell to perform electrolysis, thereby obtaining anode gas and cathode deposits of rare earths after electrolysis; S2. generating a compensation signal for secondary electrolysis of the rare earth according to the component ratio of the anode gas; S3, adding a compensating agent to the molten electrolyte according to the compensation signal to generate a regenerated electrolyte system of the rare earth; S4, generating an impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system; S5. Applying a pulse current to the rare earth based on the impedance correction parameter to obtain the impurity-removed rare earth.

[0068] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention.

[0069] The embodiments of the present application can acquire and process relevant data based on artificial intelligence technology. Artificial intelligence refers to the theories, methods, technologies, and application systems that use digital computers or machines controlled by digital computers to simulate, extend, and expand human intelligence, perceive the environment, acquire knowledge, and use knowledge to achieve optimal results.

[0070] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not limiting. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention.

Claims

1. A rare earth electrolysis device for reducing non-metallic impurities, characterized in that: The device includes an electrolysis module, a compensation signal generation module, a regeneration electrolyte system acquisition module, an impedance correction parameter generation module and a pulse impurity removal module, wherein: The electrolysis module is used to apply an initial current density to the electrolytic cell to perform electrolysis, thereby obtaining anode gas and cathode deposits of rare earths after electrolysis; The compensation signal generating module is used to generate a compensation signal for secondary electrolysis of the rare earth according to the component ratio of the anode gas; The regenerative electrolyte system acquisition module is used to add a compensating agent to the molten electrolyte according to the compensation signal to generate the regenerative electrolyte system of the rare earth; The impedance correction parameter generating module is used to generate the impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system; The pulse de-doping module is used to apply a pulse current to the rare earth based on the impedance correction parameter to obtain the de-doped rare earth.

2. The rare earth electrolysis device for reducing non-metallic impurities according to claim 1, characterized in that: The initial current density comprises: Generate a baseline value based on the initial conductivity of the electrolyte; The reference value is matched with a preset current density comparison table to obtain the initial current density of the electrolytic cell.

3. The rare earth electrolysis device for reducing non-metallic impurities according to claim 1, characterized in that: When the compensation signal generating module generates a compensation signal for secondary electrolysis of the rare earth according to the component ratio of the anode gas, the compensation signal generating module is specifically used to: detecting a volume ratio of hydrogen fluoride to carbon dioxide in the anode gas; When the volume ratio exceeds a preset threshold, a compensation signal for the electrolytic cell is generated.

4. The rare earth electrolysis device for reducing non-metallic impurities according to claim 1, characterized in that: When the regeneration electrolyte system acquisition module adds a compensating agent to the molten electrolyte according to the compensation signal to generate the rare earth regeneration electrolyte system, it is specifically used to: adding an alkali metal carbonate to the molten electrolyte according to a compensator type in the compensation signal; The electrolysis temperature is maintained within a preset time, and the rare earth carbonate precipitate is removed by filtration to obtain a regenerated electrolyte system of the rare earth.

5. The rare earth electrolysis device for reducing non-metallic impurities according to claim 1, characterized in that: When the impedance correction parameter generation module generates the impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system, the module is specifically configured to: Applying a sinusoidal current between the cathode deposit of the electrolytic cell and the regeneration electrolyte system to generate an electrode interface response signal of the rare earth; The voltage and current phase differences and amplitude ratios of the electrode interface response signals at different frequencies are collected as cathode interface impedance spectrum data of the rare earth; Fitting an equivalent circuit model to the rare earth based on the cathode interface impedance spectrum data to obtain a resistance value of the rare earth; According to the change rate of the resistance value and the initial resistance value, a preset impedance correction coefficient mapping table is matched to obtain the impedance correction coefficient of the rare earth.

6. The rare earth electrolysis device for reducing non-metallic impurities according to claim 5, characterized in that: When performing equivalent circuit model fitting on the rare earth based on the cathode interface impedance spectrum data to obtain the resistance value of the rare earth, the impedance correction parameter generation module is specifically used to: Construct a three-element equivalent circuit model; Inputting the cathode interface impedance spectrum data into the three-element equivalent circuit model and performing linear fitting; The fitting parameter value of the charge transfer resistance element in the three-element equivalent circuit model after linear fitting is extracted as the resistance value of the rare earth.

7. The rare earth electrolysis device for reducing non-metallic impurities according to claim 5, characterized in that: When the impedance correction parameter generation module performs matching of a preset impedance correction coefficient mapping table according to the change rate of the resistance value and the initial resistance value to obtain the impedance correction coefficient of the rare earth, it is specifically used to: Obtaining a baseline resistance value during the initial electrolysis stage; determining a rate of change of the resistance value according to a ratio of the resistance value to the reference resistance value; The change rate is input into a preset impedance correction coefficient mapping table, and an impedance correction coefficient linearly corresponding to the change rate is output.

8. The rare earth electrolysis device for reducing non-metallic impurities according to claim 1, characterized in that: When the pulse impurity removal module applies a pulse current to the rare earth based on the impedance correction parameter to obtain the impurity-removed rare earth, it is specifically used to: Dynamically adjusting the peak current density of the pulse current according to the impedance correction parameter; applying a pulse sequence to the cathode of the electrolytic cell with the adjusted sell power parameters; After completing the preset pulse cycle, the impurity-removed rare earth is obtained.

9. The rare earth electrolysis device for reducing non-metallic impurities according to claim 1, characterized in that: When the pulse impurity removal module dynamically adjusts the peak current density of the pulse current according to the impedance correction parameter, the calculation formula of the peak current density is as follows: Where, is the peak current density, is the cathode reaction activation factor, is the mass of cathode deposit, is the impedance correction factor, is the duration of a single pulse; The output current is dynamically adjusted according to the peak current density.

10. A rare earth electrolysis method for reducing non-metallic impurities, characterized in that: The method comprises: S1. Applying an initial current density to the electrolytic cell to perform electrolysis, thereby obtaining anode gas and cathode deposits of rare earths after electrolysis; S2. generating a compensation signal for secondary electrolysis of the rare earth according to the component ratio of the anode gas; S3, adding a compensating agent to the molten electrolyte according to the compensation signal to generate a regenerated electrolyte system of the rare earth; S4, generating an impedance correction parameter of the rare earth according to the cathode interface impedance of the regenerative electrolyte system; S5. Applying a pulse current to the rare earth based on the impedance correction parameter to obtain the impurity-removed rare earth.

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