Detection device and recovery system

Abstract

The utility model provides a detection device and a recovery system, the detection device comprises a sampling module, the sampling module comprises a sampling container, and the sampling container is used for obtaining a sampling solution from a to-be-detected solution; the dilution module comprises a dilution container, a dilution part and a transfer part, the dilution container can obtain a sampling solution, the dilution part is used for diluting the sampling solution, and the transfer part can transfer the diluted sampling solution to the detection module; the detection module is used for detecting the concentration of the set ions in the sampling liquid in real time, that is, sampling, dilution and detection are integrated, so that the structure of the detection device is simplified, and the real-time performance and accuracy of the concentration detection of the set ions in the sampling liquid are ensured.

Description

Technical Field

[0001] This utility model belongs to the field of ion concentration detection technology. Specifically, this utility model relates to a detection device and a recovery system. Background Technology

[0002] In the field of ion concentration detection, especially in the battery recycling process, battery recycling solutions often contain a variety of metal ions, and the extraction efficiency of metal ions is crucial.

[0003] The detection equipment in related technologies has many problems. On the one hand, in order to achieve high-precision online monitoring, the structure of the detection equipment is often complex, which increases the difficulty of operation and maintenance costs. On the other hand, the detection equipment with a simplified structure is difficult to guarantee the real-time performance and accuracy of monitoring. Utility Model Content

[0004] One objective of this invention is to provide a new technical solution for a detection device and a recycling system.

[0005] According to a first aspect of the present invention, a detection device is provided, the detection device comprising:

[0006] A sampling module, comprising a sampling container for obtaining a sample solution from the solution to be tested;

[0007] The system includes a dilution module and a detection module. The dilution module comprises a dilution container, a dilution component, and a transfer component. The dilution container is capable of acquiring the sample solution, the dilution component is used to dilute the sample solution, and the transfer component is capable of transferring the diluted sample solution to the detection module.

[0008] The detection module is used to detect the concentration of a set ion in the sample solution in real time.

[0009] Optionally, the detection module includes a detection component and a sample storage component;

[0010] The sample storage component is used to store the sample solution, and the detection component can detect the concentration of a set ion in the sample solution through a detection probe;

[0011] The sampling solution includes battery material recovery solution.

[0012] Optionally, the detection component is an AAS detection component, a fluorescence spectroscopy component, or an ICP-AES detection component.

[0013] Optionally, the transfer component includes at least one of a first trace sampler and a microsyringe, the transfer component being used to transfer the diluted sample solution to the sample storage component.

[0014] Optionally, the sampling module includes a driving component, the sampling container includes a sampling tube and a piston rod, one end of the sampling tube is used to obtain a sample liquid from the solution to be tested, the other end of the sampling tube has an opening, and the piston rod is connected to the opening;

[0015] The drive component is connected to the piston rod and is used to drive the piston rod to move along the opening to adjust the vacuum level in the sampling tube.

[0016] Optionally, the driving component includes a motor, a threaded rod, and a sliding component, wherein the output end of the motor is connected to the threaded rod and is capable of driving the threaded rod to rotate;

[0017] The threaded rod is connected to the piston rod via the sliding component, so that the sliding component and the piston rod move synchronously.

[0018] Optionally, the sampling module includes a sampling pipeline, one end of which is connected to an infusion pipeline for delivering the solution to be tested, and the other end of which forms a sampling port, and one end of the sampling tube is connected to the sampling port;

[0019] The sampling pipeline is equipped with a first control valve and a filter element. The first control valve is used to control the opening and closing of the sampling pipeline, and the filter element is used to filter the sampling liquid flowing in the sampling pipeline.

[0020] Optionally, it also includes a waste liquid container, wherein the sampling port is provided with a second control valve, and the waste liquid container is connected to the second control valve through a waste liquid pipeline.

[0021] Optionally, it also includes a washing container, and the sampling tube is provided with a third control valve;

[0022] The washing container is connected to the third control valve via a washing pipeline.

[0023] Optionally, a fourth control valve is provided on the sampling tube, and a sample line is provided between the sampling tube and the dilution container. The fourth control valve is located in the sample line and is used to control the on / off state of the sample line.

[0024] Optionally, the system further includes a first converter having a first port, a second port, a third port, and a fourth port that are interconnected. The first port is connected to the dilution container, the second port is connected to the transfer component, the third port is connected to the detection module, and the fourth port is connected to the washing container.

[0025] Optionally, it also includes a second converter having a fifth port, a sixth port, and a sampling port that are interconnected.

[0026] The dilution component includes a dilution tank and a sampling device. The fifth port is connected to the inside of the dilution container, the sixth port is connected to the dilution tank, and the sampling port is connected to the sampling device.

[0027] Optionally, the sampling device includes a second trace sampler and a micro sampler, wherein the sampling accuracy of the micro sampler is higher than that of the second trace sampler;

[0028] The sampling ports include a seventh port and an eighth port, and the seventh port and the eighth port are connected to the fifth port and the sixth port in pairs; the seventh port is connected to the second trace sampler, and the eighth port is connected to the micro sampler.

[0029] According to a second aspect of the present invention, a recycling system is provided, the recycling system comprising an infusion pipeline and the detection device described in the first aspect;

[0030] The infusion line is used to deliver the solution to be tested, and the sampling container is connected to the infusion line.

[0031] One technical advantage of this utility model is:

[0032] This application provides a detection device, which includes a sampling module, a sampling container for obtaining a sample solution from a solution to be tested; a dilution module and a detection module. The dilution module includes a dilution container, a dilution component, and a transfer component. The dilution container can obtain the sample solution, the dilution component is used to dilute the sample solution, and the transfer component can transfer the diluted sample solution to the detection module. The detection module is used to detect the concentration of a set ion in the sample solution in real time. That is, sampling, dilution, and detection are integrated into one unit, simplifying the structure of the detection device and ensuring the real-time performance and accuracy of the detection of the set ion concentration in the sample solution.

[0033] Other features and advantages of the present invention will become clear from the following detailed description of exemplary embodiments of the present invention with reference to the accompanying drawings. Attached Figure Description

[0034] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments of the present invention and, together with their description, serve to explain the principles of the present invention.

[0035] Figure 1 This is a schematic diagram of a detection device provided in one embodiment of the present invention.

[0036] in:

[0037] 100. Detection device; 1. Sampling module; 11. Sampling container; 111. Sampling tube; 112. Piston rod; 113. Third control valve; 114. Fourth control valve; 12. Drive component; 121. Motor; 122. Threaded rod; 123. Sliding component; 13. Sampling pipeline; 131. First control valve; 132. Filter component; 133. Second control valve; 2. Dilution module; 21. Dilution container; 22. Dilution component; 221. Dilution tank; 222. Second trace sampler; 223. Micro sampler; 23. Transfer component; 3. Detection module; 31. Detection component; 32. Sample storage component; 321. Sample rack; 322. Sample tube; 33. Detection probe; 4. Waste liquid container; 5. Washing container; 6. First converter; 7. Second converter; 8. Electrical control module; 9. Gas storage container; 10. Buffer base;

[0038] 200. Infusion tubing; 300. Control device; 400. Display device. Detailed Implementation

[0039] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that, unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps set forth in these embodiments do not limit the scope of the present invention.

[0040] The embodiments of this application will now be described in detail, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this application, and should not be construed as limiting this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0041] The terms "first" and "second" in the specification and claims of this application may explicitly or implicitly include one or more of the features. In the description of this application, unless otherwise stated, "multiple" means two or more. Furthermore, "and / or" in the specification and claims indicates at least one of the connected objects, and the character " / " generally indicates that the preceding and following objects are in an "or" relationship.

[0042] In the description of this application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application.

[0043] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection between two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.

[0044] It should be noted that similar labels and letters in the following figures indicate similar items; therefore, once an item is defined in one figure, it does not need to be discussed further in subsequent figures.

[0045] Reference Figure 1 This application provides a detection device for detecting the concentration of ions in a solution. The detection device includes:

[0046] Sampling module 1 includes sampling container 11, which is used to obtain sampling liquid from the solution to be tested;

[0047] The dilution module 2 includes a dilution container 21, a dilution component 22, and a transfer component 23. The dilution container 21 can acquire the sample liquid, the dilution component 22 is used to dilute the sample liquid, and the transfer component 23 can transfer the diluted sample liquid to the detection module 3.

[0048] The detection module 3 is used to detect the concentration of a set ion in the sample solution in real time.

[0049] In this embodiment, the sampling module 1 is used to obtain a sample solution from the solution to be tested. The solution to be tested can be the recovery solution from different process stages in the battery recycling process or other solutions to be tested. For example, the solution in the wet recycling line of lithium iron phosphate battery can be sampled directly through the sampling container 11 of the sampling module 1 to quickly obtain the sample solution in the battery recycling solution, which provides convenience for the subsequent analysis and detection of the sample solution.

[0050] See Figure 1 The dilution container 21 of the dilution module 2 can hold the sample solution. The dilution component 22 can dilute the sample solution by adding diluent or adjusting the solution volume, such as diluting the sample solution according to a predetermined ratio or concentration, so that the concentration of the ions to be detected in the sample solution is within the measurable concentration range, ensuring the accuracy and reliability of the detection results. The transfer component 23 can transfer the diluted sample solution to the detection module 3, avoiding errors and inconveniences of manual operation and improving work efficiency.

[0051] See Figure 1 The detection module 3 can detect the concentration of the specified ions in the sample solution in real time. This real-time capability makes the detection process faster and provides timely results, facilitating the timely processing of the test solution. For example, if the detection module 3 detects a high concentration of the specified ions in the sample solution, it means that the concentration of the specified ions in the test solution is also high, indicating that the recovery efficiency of the specified ions in the test solution is low, and the specified ions in the test solution can continue to be recovered. Conversely, if the detection module 3 detects a low concentration of the specified ions in the sample solution, such as when the concentration of the specified ions in the sample solution is below the recovery standard, it means that the concentration of the specified ions in the test solution is also low, indicating that the recovery efficiency of the specified ions in the test solution is high, and the test solution can be treated as waste liquid.

[0052] In this embodiment, when the concentration of a set ion in the recycled liquid during the battery recycling process is detected by the detection device, the set ion can be lithium ion, copper ion, iron ion, nickel ion, cobalt ion or manganese ion. The above ions can be recycled separately through different process lines or uniformly through the same process line. This application embodiment does not limit this.

[0053] It is worth noting that the dilution component 22 of the dilution module 2 is used to dilute high-concentration sample solutions. For example, when the lithium ion concentration in the test solution is higher than the range of the detection module 3, the sample solution can be diluted by the dilution component 22 to ensure that the detection module 3 can detect the concentration of the set ions in the sample solution in real time. When the lithium ion concentration in the test solution is within the range of the detection module 3, the sample solution may not be diluted; instead, the transfer component 23 can directly transfer the sample solution in the dilution container 21 to the detection module 3.

[0054] In this embodiment, the detection module 3 can monitor the residual concentration of ions in the test solution in real time. While ensuring the purity of the recovered ions, it can effectively control the residual ions in the test solution, avoid the waste of ions in the test solution, and ensure the ion recovery efficiency.

[0055] The detection device provided in this application includes a sampling module 1, which includes a sampling container 11 for obtaining a sample solution from the solution to be tested; a dilution module 2 and a detection module 3. The dilution module 2 includes a dilution container 21, a dilution component 22, and a transfer component 23. The dilution container 21 can obtain the sample solution, the dilution component 22 is used to dilute the sample solution, and the transfer component 23 can transfer the diluted sample solution to the detection module 3. The detection module 3 is used to detect the concentration of a set ion in the sample solution in real time. That is, sampling, dilution and detection are integrated into one unit. The real-time online monitoring of the concentration of the set ion in the sample solution is realized through a fully automatic device, which simplifies the structure of the detection device and ensures the real-time performance and accuracy of the detection of the set ion concentration in the sample solution.

[0056] In some embodiments, see Figure 1 The detection module 3 includes a detection component 31 and a sample storage component 32;

[0057] The sample storage component 32 is used to store the sample solution, and the detection component 31 can detect the concentration of a set ion in the sample solution through the detection probe 33;

[0058] The sampling fluid includes recycled battery material fluid.

[0059] In this embodiment, the sampling liquid includes battery material recovery liquid, which can be lithium iron phosphate battery material recovery liquid. Lithium iron phosphate battery materials do not contain heavy metals such as nickel, cobalt, and manganese, while lithium in lithium iron phosphate batteries has high recycling value. The detection component 31 detects lithium ions in the lithium iron phosphate battery material recovery liquid through the detection probe 33, which can specifically recover lithium as a single element in the recovery liquid. The technology is low and the recycling process is simple.

[0060] Specifically, after the lithium iron phosphate battery material is mechanically crushed, black powder is separated. The black powder is then leached with strong acids such as sulfuric acid and hydrogen peroxide, which dissolves lithium elements in ionic form in the solution, while iron ions precipitate as iron phosphate. Subsequently, lithium ions in lithium sulfate can be separated as lithium carbonate by adding carbonates such as sodium carbonate and sodium hydroxide. After separation, the concentration of lithium ions in the remaining sodium sulfate in the solution can be detected by the detection component 31 to ensure the recovery efficiency and purity of lithium elements.

[0061] In this embodiment, the detection probe 33 can accurately measure the sample solution from the sample tube and transfer the sample solution to the detection component 31 for detection. The detection component 31 can efficiently and accurately detect lithium ions in the sample solution.

[0062] In some embodiments, the detection component 31 is an AAS detection component, a fluorescence spectroscopy component, or an ICP-AES detection component.

[0063] In this embodiment, the AAS (Atomic Absorption Spectroscopy) detection component performs measurements based on the absorption of light at a specific wavelength by ions. Specifically, ions in the sample are vaporized and then atomized by a flame or other atomizer, producing a series of excited-state atoms. These excited-state atoms absorb light at a specific wavelength, thus generating an absorption peak. The intensity of the absorbed light is proportional to the concentration of ions in the sample; therefore, the ion concentration can be determined by comparing the sample's absorbed light intensity with a standard curve.

[0064] Fluorescence spectroscopy components are used in atomic fluorescence spectrometry (AFS) analysis. Fluorescence spectroscopy is based on the emission of fluorescence when gaseous free atoms absorb radiation from a characteristic light source, causing their outer electrons to transition to higher energy levels and then back to the ground or lower energy levels. A detector captures the fluorescence signal and converts it into an electrical signal for recording and analysis. Based on the intensity and characteristic wavelength of the fluorescence signal, the types and concentrations of ions in the solution can be determined efficiently and accurately.

[0065] The ICP-AES detection unit converts the sample solution into an aerosol via argon atomization. In a plasma torch, the sample aerosol is excited by high temperature, causing electrons in the atoms to transition from lower to higher energy levels. When the electrons fall back to the lower energy levels, element-specific electromagnetic rays are emitted. These emission spectra are dispersed using a diffraction grating, and the intensity of light at each wavelength is measured using a charge-coupled device (CCD) detector. Based on the unique emission spectrum and intensity of each element, the type and concentration of ions in the solution can be determined, minimizing matrix effects and ionization interference, and improving the accuracy and reliability of detection.

[0066] In one embodiment, the sample storage component 32 includes a sample rack 321 and sample tubes 322, with multiple sample tubes 322 arranged on the sample rack 321 and used to receive and store sample solutions transferred from the dilution container 21.

[0067] The AAS detection component has high selectivity and sensitivity, enabling accurate measurement of the concentration of specific metal ions such as lithium ions. Moreover, the equipment cost is lower than that of ICP-OES equipment, realizing online monitoring of lithium ion concentration.

[0068] In some embodiments, the transfer component 23 includes at least one of a first trace sampler and a microsyringe, and the transfer component 23 is used to transfer the diluted sample solution to the sample storage component 32.

[0069] In this embodiment, the sampling accuracy of the first trace sampler is hundreds of microliters, while the sampling accuracy of the microsyringe is microliters. That is, the sampling accuracy of the microsyringe is higher than that of the first trace sampler, which can bring high-precision sampling and transfer, reduce sample contamination and loss, and improve detection efficiency.

[0070] In one specific embodiment, the sampling container 11 is used to extract from... Figure 1 A sample is taken from the sodium sulfate filtrate after lithium precipitation at point 200 in the liquid infusion line. After the sample is diluted and brought to volume, 10 mL of the diluted sample is drawn into the sample tube 322 by the first trace sampler for testing.

[0071] After the sample solution in the dilution container 21 is back-transferred, the first trace sampler can draw up the washing solution to wash the tubing and dilution container 21 multiple times, and then inject the washed solution into the sample tube 322 for testing to ensure the cleanliness of the dilution container 21.

[0072] In some embodiments, see Figure 1 The sampling module 1 includes a driving component 12, and the sampling container 11 includes a sampling tube 111 and a piston rod 112. One end of the sampling tube 111 is used to obtain the sampling liquid from the solution to be tested, and the other end of the sampling tube 111 has an opening, and the piston rod 112 is connected to the opening.

[0073] The drive component 12 is connected to the piston rod 112 and is used to drive the piston rod 112 to move along the opening to adjust the vacuum level in the sampling tube 111.

[0074] In this embodiment, the driving component 12 can be a driving motor or a cylinder, etc. When the driving component 12 is a driving motor, when the driving motor drives the piston rod 112 to move away from the sampling tube 111 along the opening, the vacuum degree can be increased by increasing the space inside the sampling tube 111. The solution to be tested is in a normal pressure or pressurized pipeline, and the solution to be tested can flow into the sampling tube 111 under the action of pressure difference, so as to realize negative pressure sampling of the sampling tube 111.

[0075] Furthermore, by precisely controlling the piston rod 112 through the drive component 12, the vacuum level inside the sampling tube 111 can be accurately adjusted, thereby accurately controlling the sampling amount and improving the accuracy and reliability of sampling.

[0076] When the sampled liquid in the sampling tube 111 needs to be transported to the dilution container 21, the piston rod 112 can be driven by the drive motor to move along the opening towards the sampling tube 111, so as to increase the pressure inside the sampling tube 111 by reducing the space inside the sampling tube 111. Since the internal space of the dilution container 21 is at normal pressure, the sampled liquid can flow into the dilution container 21 under the action of pressure difference.

[0077] See Figure 1 One end of the sampling tube 111 is directly inserted into the solution to be tested to obtain the sample liquid, and the other end of the sampling tube 111 is connected to the driving component 12 through the piston rod 112, which avoids external air or impurities from entering the sampling tube 111 during the sampling process, thereby reducing the risk of the sample liquid being contaminated.

[0078] Alternatively, when cleaning the sampling tube 111, the cleaning fluid can be drawn into the sampling tube 111 by negative pressure cleaning, and the cleaning fluid can be discharged from the sampling tube 111 by pressurization after cleaning.

[0079] In some embodiments, see Figure 1 The driving component 12 includes a motor 121, a threaded rod 122 and a sliding component 123. The output end of the motor 121 is connected to the threaded rod 122 and can drive the threaded rod 122 to rotate.

[0080] The threaded rod 122 is connected to the piston rod 112 via the sliding member 123, so that the sliding member 123 and the piston rod 112 move synchronously.

[0081] In this embodiment, the motor 121 transmits rotational power to the threaded rod 122 via its output shaft or through a transmission device such as a reducer. The reducer can be implemented using a coupling, gear, or belt to ensure the effective rotation of the threaded rod 122. The axial direction of the threaded rod 122 is parallel to the extension direction of the piston rod 112. The threaded rod 122 engages with a nut or a sliding component 123 with internal threads to form a threaded connection between the threaded rod 122 and the sliding component 123. When the threaded rod 122 rotates, the sliding component 123 moves along the axial direction of the threaded rod 122, thereby achieving synchronous linear movement of the sliding component 123 and the piston rod 112, thus improving the stability and efficiency of sampling.

[0082] In some embodiments, see Figure 1 The sampling module 1 includes a sampling pipeline 13, one end of which is connected to the infusion pipeline 200 for conveying the solution to be tested, and the other end of the sampling pipeline 13 forms a sampling port. One end of the sampling tube 111 is connected to the sampling port.

[0083] The sampling pipeline 13 is equipped with a first control valve 131 and a filter element 132. The first control valve 131 is used to control the opening and closing of the sampling pipeline 13, and the filter element 132 is used to filter the sampling liquid flowing in the sampling pipeline 13.

[0084] In the above embodiment, during the process of sampling the sample liquid from the solution to be tested to the sampling tube 111, the sampling tube 13 is precisely controlled by the first control valve 131 to achieve accurate sampling of the solution to be tested in the infusion tube 200. For example, the parameters such as sampling position, sampling amount and sampling frequency are adjusted to ensure the reliability of subsequent analysis or testing.

[0085] The filter element 132 effectively removes impurities and insoluble substances such as particulate matter from the sampling liquid flowing in the sampling tube 13. This ensures a high-purity and clean sampling liquid, avoids the influence of impurities on the ion concentration test results in the sampling liquid, and prevents impurities from clogging the sampling tube 111.

[0086] In some embodiments, see Figure 1 The detection device also includes a waste liquid container 4, and a second control valve 133 is provided at the sampling port. The waste liquid container 4 is connected to the second control valve 133 through a waste liquid pipeline.

[0087] In this embodiment, the waste liquid remaining in the sampling tube 111 and sampling pipeline 13 can be collected, stored and treated by the waste liquid container 4. The precise control of the second control valve 133 makes the discharge of waste liquid more flexible and efficient.

[0088] Waste liquid generated in sampling tube 111 and sampling pipeline 13 during sampling or testing can be directly discharged into waste liquid container 4 through waste liquid pipeline when the second control valve 133 is opened, thus avoiding random discharge of waste liquid and pollution to the environment.

[0089] In some embodiments, see Figure 1 The detection device also includes a washing container 5 and a third control valve 113 on the sampling tube 111;

[0090] The washing container 5 is connected to the third control valve 113 via a washing pipeline.

[0091] In this embodiment, the third control valve 113 controls the opening and closing of the washing pipeline between the washing container 5 and the sampling tube 111. The sampling tube 111 can be washed before sampling, for example, by creating a vacuum in the sampling tube 111 and using pressure difference to force the washing liquid in the washing container 5 into the sampling tube 111 to remove residues or contaminants in the sampling tube 111, ensuring the cleanliness of the sampling tube 111, which helps to improve the accuracy of sampling and avoid the influence of residues on the sampling results.

[0092] In some embodiments, see Figure 1 A fourth control valve 114 is provided on the sampling tube 111. A sample line is provided between the sampling tube 111 and the dilution container 21. The fourth control valve 114 is provided on the sample line and is used to control the opening and closing of the sample line.

[0093] In this embodiment, the fourth control valve 114 is disposed in the sample tubing and used to control the opening and closing of the sample tubing. When the sample liquid in the sampling tube 111 needs to be transferred to the dilution container 21, the fourth control valve 114 can be used to open the sample tubing to realize the transfer of the sample liquid before dilution. After the sample liquid is transferred to the dilution container 21, the fourth control valve 114 can be closed to disconnect the sample tubing, preventing the liquid in the sample tubing from flowing back to the sampling tube 111. This ensures that the sample liquid is fully diluted while avoiding cross-contamination caused by the backflow of the sample liquid.

[0094] It is worth noting that each control valve mentioned in the embodiments of this application can be controlled individually to ensure precise control of sampling, detection and cleaning, thereby improving the adaptability and flexibility of the detection device.

[0095] In some embodiments, see Figure 1 The detection device also includes a first converter 6, which has a first port, a second port, a third port and a fourth port that are interconnected. The first port is connected to the dilution container 21, the second port is connected to the transfer component 23, the third port is connected to the detection module 3 and the fourth port is connected to the washing container 5.

[0096] In this embodiment, the first converter 6 and the pipeline connected thereto form a transmission module. The pipeline on the transmission module can be made of PTFE (Polytetrafluoroethylene). The first converter 6 can be a multi-port valve to achieve pipeline optimization and automation of sample transmission and processing.

[0097] The multi-port design of the first converter 6 allows multiple operation steps to be performed simultaneously or sequentially. For example, after the transfer component 23 transfers the sample liquid in the dilution container 21 to the detection module 3, the dilution container 21 can be washed in time by the washing container 5, which shortens the time required for the entire detection process and improves detection efficiency.

[0098] In some embodiments, see Figure 1 The detection device also includes a second converter 7, which has a fifth port, a sixth port and a sampling port that are interconnected.

[0099] The dilution component 22 includes a dilution tank 221 and a sampling device. The fifth port is connected to the inside of the dilution container 21, the sixth port is connected to the dilution tank 221, and the sampling port is connected to the sampling device.

[0100] In this embodiment, the fifth port, the sixth port, and the sampling port can be connected in pairs so that the diluent in the dilution tank 221 can be injected into the sampling liquid in the dilution container 21 through the sampling device to realize the dilution operation of the sampling liquid. The diluted sampling liquid is injected into the sample tube 322, sampled by the detection probe 33 of the detection component 31, and transported into the detection component 31 for detection to ensure the accuracy and precision of dilution.

[0101] In some embodiments, see Figure 1 The sampling device includes a second trace sampler 222 and a micro sampler 223. The sampling accuracy of the micro sampler 223 is higher than that of the second trace sampler 222.

[0102] The sampling ports include a seventh port and an eighth port, which are connected to the fifth port and the sixth port in pairs; the seventh port is connected to the second trace sampler 222, and the eighth port is connected to the micro sampler 223.

[0103] In this embodiment, the sample liquid in the dilution container 21 can be accurately diluted by injecting diluent through the second trace sampler 222 and the micro sampler 223. The diluted sample liquid is injected into the sample tube 322, sampled by the detection probe 33 of the detection component 31 and transported into the detection component 31 for detection. The combined sampling by the second trace sampler 222 and the micro sampler 223 can ensure the precision and accuracy of dilution.

[0104] Specifically, when the sample liquid in the dilution container 21 is diluted, the electrical control module 8 of the detection device determines the volume of the sample liquid and opens the seventh and sixth ports connected to the second trace sampler 222 and the dilution tank 221. The second trace sampler 222 first samples the diluent from the dilution tank 221. The sampling accuracy of the second trace sampler 222 is 100 microliters. Then, the sixth port is closed and the fifth port is opened to inject the diluent from the second trace sampler 222 into the dilution container 21.

[0105] Then, the eighth and sixth ports connected to the micro sampler 223 and the dilution container 221 are opened, and the micro sampler 223 takes a sample through the second converter 7. The sampling accuracy of the micro sampler 223 is microliters. Then the sixth port is closed and the fifth port is opened, and the diluent in the micro sampler 223 is injected into the dilution container 21 to complete the dilution and volume adjustment of the sampled liquid in the dilution container 21.

[0106] In another embodiment, the sampling device includes two or more second trace samplers 222 to increase the sampling amount of the sampling device; in yet another embodiment, the sampling device includes two or more micro samplers 223 to improve the sampling accuracy of the sampling device while ensuring the sampling amount of the sampling device.

[0107] In one embodiment, see Figure 1 The testing device also includes an electrical control module 8, which controls the opening and closing of each control valve and the operation of the motor. Specifically, the electrical control module 8 uses control signals to start, stop, and adjust each control valve and the motor, ensuring the stability of the entire testing device.

[0108] In one embodiment, see Figure 1 The detection device also includes a gas storage container 9, which stores acetylene gas and is connected to the detection module 3. Acetylene gas has the characteristics of high temperature, high calorific value and high purity, making it suitable for the atomization process in AAS analysis.

[0109] In one specific embodiment, acetylene gas is stored in a compressed gas cylinder, with a cylinder size of 40L or 50L and a pressure of 15MPa. To ensure the stability and accuracy of the atomization process, the purity of the acetylene gas is required to be above 99.9%, and it undergoes purification and drying treatment.

[0110] During the detection of ion concentration by the detection component 31, high-temperature acetylene gas is generated. This high-temperature gas may adversely affect the detection equipment and process. The condenser in the detection component 31 transfers heat from the high-temperature gas to the outside through its heat exchange function, thereby reducing the gas temperature and ensuring the normal detection of the detection module.

[0111] In one specific embodiment, the detection process of the detection device includes the following steps:

[0112] S101, during the sampling phase of the sampling module, the electrical control module controls the opening of the first control valve, while the second, third, and fourth control valves are closed. At this time, the electrical control module controls the motor to rotate and drives the piston rod to move upward, causing the piston, which was originally in a neutral position inside the sampling tube, to move upward. This creates a negative pressure inside the sampling tube, allowing the sampling liquid to enter the sampling tube through the sampling pipeline via the first control valve.

[0113] S102, the fourth control valve is opened, and the motor controls the piston rod to move downward, so that positive pressure is formed in the sampling tube. The sampling liquid in the sampling tube is transported to the dilution container 21 through the positive pressure. The sampling liquid is diluted in the dilution container 21. The amount of diluent transported during the dilution operation is accurately measured by the liquid flow meter and fed back to the electrical control module, so as to control the motor to rotate and stop through the electrical control module.

[0114] S103, the electrical control module controls the fourth control valve to close and the second control valve to open. The motor controls the piston rod to move downward, conveying the excess sampling liquid in the sampling tube to the waste liquid container under positive pressure. Then, the electrical control module controls the second control valve to close and the third control valve to open. The motor controls the piston rod to move upward, drawing the washing liquid in the washing container into the sampling tube under negative pressure. Finally, the washing liquid after washing is discharged into the waste liquid container as waste liquid by opening the second control valve again.

[0115] The step of detecting the ion concentration by the detection component 31 can be between steps S102 and S103, or after step S103.

[0116] After the detection device completes the ion concentration detection, it can discharge the sample solution in the detection cell of the detection module 3 and wash the pipeline by controlling the pressure in the sampling tube and the opening and closing of the second, third and fourth control valves. The cleaning process can be fully automatically controlled and the cleaning operation is convenient and quick.

[0117] In one embodiment, see Figure 1 The detection device also includes a buffer base 10. The detection device 100 includes a cabinet, inside which a sampling module 1, a dilution module 2 and a detection module 3 are installed. The buffer base 10 is located at the bottom of the cabinet.

[0118] In this embodiment, the buffer base 10, based on the elastic deformation capability of the spring, can absorb and buffer vibration energy through the internal spring structure when the detection device is subjected to vibration, thereby reducing the impact and damage of vibration on the detection device and internal pipes.

[0119] This application embodiment also provides a recycling system, which includes an infusion pipeline 200 and the detection device 100 described above;

[0120] The infusion line 200 is used to deliver the solution to be tested, and the sampling container 11 is connected to the infusion line 200 and used to obtain the sample solution from the solution to be tested.

[0121] In this embodiment, the recovery system also includes a control device 300 and a display device 400. The control device 300 can receive signals sent by the electrical control module 8 and control valve opening and closing, motor rotation, condenser temperature setting, and release of compressed gas in the gas storage container through the electrical control module 8.

[0122] In addition, the electrical control module 8 can process, analyze, record, and store the detection data, and the display panel of the display device 400 can output the results.

[0123] The present application will be further described in detail below through examples, taking the monitoring of lithium ion concentration in lithium iron phosphate battery material recovery liquid as an example.

[0124] First, the relationship between lithium-ion concentration and AAS absorbance values ​​was calibrated. A series of lithium-ion solutions with gradient concentrations (0.1, 0.5 ppm, 1 ppm, 2 ppm, 10 ppm, 20 ppm, 50 ppm, 100 ppm) were prepared. By measuring the absorbance intensity of the AAS atomic absorption spectrometer, the linear calibration formula for the relationship between absorbance and lithium-ion concentration was obtained as follows:

[0125] y = 0.206x + 0.008

[0126] Where y is absorbance and x is lithium ion concentration, in ppm.

[0127] Secondly, black powder from crushed waste lithium iron phosphate batteries is leached with acid to obtain a black powder solution. Then, insoluble iron phosphate is removed by solid-liquid separation filtration. Sodium carbonate and sodium hydroxide are added to the lithium sulfate filtrate to precipitate lithium, followed by another solid-liquid separation, and the filtrate is collected.

[0128] The filtrate is sampled using the detection device of this embodiment. The sampling tube has an inner diameter of 3.0 mm, and the single sampling volume is 10 mL. 5 mL of the sample is transferred to the dilution container, and the remaining sample is transferred to the waste container. The second trace sampler draws diluent to dilute the sample by one-fold. The diluted sample in the dilution container is then injected into the sample tube via the second converter through the trace sampler.

[0129] The sample was tested and the absorbance was 0.799, indicating that the lithium ion concentration was 3.84 ppm, which conforms to the above linear calibration formula.

[0130] Based on the detection device provided in this application embodiment, the same batch of sampled liquid recovered by wet method was sampled and measured 6 times at different times. The detection results of the above embodiment (Example 1) together with the measurement results of the other 5 embodiments (Examples 2-6) are shown in Table 1.

[0131] Table 1 Results of the embodiments of the lithium-ion online detection device of this application

[0132]

[0133] As can be seen from Table 1, the detection device provided in this application embodiment can accurately detect the ion concentration in the sample liquid, and the detection is fast and the detection results are stable.

[0134] Although specific embodiments of the present invention have been described in detail by way of examples, those skilled in the art should understand that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Those skilled in the art should understand that modifications can be made to the above embodiments without departing from the scope and spirit of the present invention. The scope of the present invention is defined by the appended claims.

Claims

1. A detection device, characterized in that, The application relates to a device for detecting the concentration of a set ion in a sample solution, comprising: a sampling module (1) comprising a sampling container (11) for obtaining a sample solution from a solution to be measured; a dilution module (2) comprising a dilution container (21) capable of obtaining the sample solution, a dilution component (22) for diluting the sample solution, and a transfer component (23) for transferring the diluted sample solution to a detection module (3); the detection module (3) is used for real-time detection of the concentration of the set ion in the sample solution.

2. The detection device of claim 1, wherein, The detection module (3) comprises a detection component (31) and a sample storage component (32); the sample storage component (32) is used for storing the sample solution, and the detection component (31) is capable of detecting the concentration of the set ion in the sample solution through a detection probe (33); the sample solution comprises a battery material recycling solution.

3. The detection device of claim 2, wherein, The detection component (31) is an AAS detection component, a fluorescence spectrum component or an ICP-AES detection component.

4. The detection device of claim 2, wherein, The transfer component (23) comprises at least one of a first trace sampler and a microinjector, and is used for transferring the diluted sample solution to the sample storage component (32).

5. The detection device of claim 1, wherein, The sampling module (1) comprises a driving component (12), the sampling container (11) comprises a sampling tube (111) and a piston rod (112), one end of the sampling tube (111) is used for obtaining the sample solution from the solution to be measured, the other end of the sampling tube (111) has an opening, and the piston rod (112) is connected to the opening; the driving component (12) is connected to the piston rod (112) and is used for driving the piston rod (112) to move along the opening so as to adjust the vacuum degree in the sampling tube (111).

6. The detection device of claim 5, wherein, The driving component (12) comprises a motor (121), a threaded rod (122) and a sliding component (123), the output end of the motor (121) is connected to the threaded rod (122) and is capable of driving the threaded rod (122) to rotate; the threaded rod (122) is connected to the piston rod (112) through the sliding component (123), so that the sliding component (123) and the piston rod (112) move synchronously.

7. The detection device of claim 5, wherein, The sampling module (1) comprises a sampling pipeline (13), one end of the sampling pipeline (13) is communicated to a liquid delivery pipeline (200) for delivering the solution to be measured, the other end of the sampling pipeline (13) forms a sampling port, and one end of the sampling tube (111) is connected to the sampling port; a first control valve (131) and a filtering device (132) are arranged on the sampling pipeline (13), the first control valve (131) is used for controlling the opening and closing of the sampling pipeline (13), and the filtering device (132) is used for filtering the sample solution flowing through the sampling pipeline (13).

8. The detection device of claim 7, wherein, Further comprising a waste liquid container (4), the sampling port is provided with a second control valve (133), the waste liquid container (4) is connected to the second control valve (133) through a waste liquid pipeline.

9. The detection device of claim 5, wherein, Further comprising a washing container (5), the sampling pipeline (111) is provided with a third control valve (113); The washing container (5) is connected to the third control valve (113) through a washing pipeline.

10. The detection device of claim 5, wherein, The sampling pipeline (111) is provided with a fourth control valve (114), a sample pipeline is arranged between the sampling pipeline (111) and the dilution container (21), and the fourth control valve (114) is arranged in the sample pipeline and is used for controlling opening and closing of the sample pipeline.

11. The detection device of claim 9, wherein, Further comprising a first switch (6), the first switch (6) has a first port, a second port, a third port and a fourth port which are in communication with each other, the first port is communicated to the inside of the dilution container (21), the second port is communicated to the transfer component (23), the third port is communicated to the detection module (3), and the fourth port is communicated to the washing container (5).

12. The detection device of claim 1, wherein, Further comprising a second switch (7), the second switch (7) has a fifth port, a sixth port and a sampling port which are in communication with each other; The dilution component (22) comprises a dilution tank (221) and a sampling device, the fifth port is communicated to the inside of the dilution container (21), the sixth port is communicated to the dilution tank (221), and the sampling port is communicated to the sampling device.

13. The detection device of claim 12, wherein, The sampling device comprises a second trace sampler (222) and a micro sampler (223), sampling precision of the micro sampler (223) is higher than that of the second trace sampler (222); The sampling port comprises a seventh port and an eighth port, the seventh port and the eighth port are in communication with the fifth port and the sixth port in pairs; the seventh port is communicated to the second trace sampler (222), and the eighth port is communicated to the micro sampler (223).

14. A recycling system characterized by, The detection device (100) comprises a liquid delivery pipeline (200) and the detection device (100) according to any one of claims 1-13. The liquid delivery pipeline (200) is used for delivering a solution to be detected, and the sampling container (11) is connected to the liquid delivery pipeline (200).

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