A measuring device and method

Abstract

The application provides a measuring device and method; the measuring device comprises: an X-ray emitter for emitting X-rays; a flow cell arranged on the light path of the X-rays, for flowing rare earth solution, the rare earth solution comprising multiple rare earth elements; a detector for detecting the emergent light after the X-rays irradiate the rare earth solution in the flow cell, generating spectral data of the emergent light; a control and data processing unit connected with the detector, for determining the transmittance corresponding to each rare earth element in the multiple rare earth elements based on the spectral data, inputting the transmittance corresponding to the multiple rare earth elements respectively into a multi-element simultaneous measurement model, and obtaining the concentration of each rare earth element in the rare earth solution; the control and data processing unit is also connected with the X-ray emitter, for adjusting the voltage parameter and the current parameter of the X-ray emitter. Through the scheme provided by the application, the concentration of multiple rare earth elements can be measured online, and the real-time regulation and control demand of the extraction separation process is met.

Description

Technical Field

[0001] This application relates to the field of rare earth element analysis technology, and in particular to a measuring device and method. Background Technology

[0002] Rare earth elements, due to their unique optical, electrical, magnetic, and catalytic physicochemical properties, are widely used in key fields such as new energy materials, high-end equipment manufacturing, metallurgy, chemical industry, and aerospace, and are a strategic key resource for the country. Different rare earth elements have similar physicochemical properties, and the various rare earth components in natural minerals and mixed solutions are often mixed, making it difficult to meet the high-purity requirements for industrial use. Therefore, the extraction and separation process of rare earth elements is a core and crucial step in the deep processing of rare earths.

[0003] To achieve high precision and purity in the extraction and separation of rare earth elements, it is necessary to determine the content of various rare earth elements in the solution. This allows for the adjustment of process parameters such as the extraction stage and liquid flow rate based on the concentration of these elements. Currently, the measurement of rare earth element content primarily relies on offline analysis, which involves manually sampling at various points within the extraction process to measure the rare earth element content. However, this offline analysis method not only requires manual operation but also suffers from a certain lag in the measurement results, making it difficult to meet the real-time control requirements of the extraction and separation process. Summary of the Invention

[0004] To address the related technical problems, embodiments of this application provide a measuring device and method.

[0005] The technical solution of this application embodiment is implemented as follows: This application provides a measuring device, which includes an X-ray emitter, a flow cell, a detector, and a control and data processing unit; wherein... The X-ray emitter is used to emit X-rays; The flow cell is disposed in the optical path of the X-ray and is used to flow a rare earth solution, wherein the rare earth solution includes a variety of rare earth elements; The detector is used to detect the emitted light after the X-rays irradiate the rare earth solution in the flow cell, and to generate spectral data of the emitted light. The control and data processing unit is connected to the detector and is used to determine the transmittance of each rare earth element among the multiple rare earth elements based on the spectral data. The transmittance of each rare earth element is input into the multi-element simultaneous measurement model to obtain the concentration of each rare earth element in the rare earth solution. The multi-element simultaneous measurement model is obtained based on the transmittance and concentration of each rare earth element in multiple solution samples, and the concentrations of the multiple rare earth elements are different in different solution samples.

[0006] In the above scheme, the control and data processing unit is further used for: Based on the concentration of each rare earth element in the rare earth solution, the proportions of one or more liquids in the rare earth feed solution, aqueous phase, and organic phase during the rare earth element extraction process are adjusted.

[0007] In the above scheme, the measuring device further includes: A filter is used to filter out X-rays emitted by the X-ray emitter that are outside the target energy range, wherein the target energy range includes the frequency band where the absorption edges of the various rare earth elements are located; A collimator is used to control the X-rays filtered by the filter to pass through the flow cell and then enter the detector.

[0008] In the above scheme, the control and data processing unit is specifically used for: Based on the spectral data, the absorption edge of each rare earth element among the various rare earth elements is determined; The transmittance of each rare earth element is determined based on its absorption edge.

[0009] In the above scheme, the spectral data represents the radiation intensity corresponding to different energies, and the control and data processing unit is specifically used for: Identify each energy region in which the ray intensity of the spectral data undergoes abrupt changes; The spectral data of each energy region is determined as the absorption edge of the rare earth element.

[0010] In the above scheme, the control and data processing unit is specifically used for: For each rare earth element, a first transmittance and a second transmittance are determined on both sides of the absorption edge of the rare earth element, wherein the first transmittance is the ratio of the first intensity before the change in radiation intensity to the initial intensity of the emitted light, and the second transmittance is the ratio of the second intensity after the change in radiation intensity to the initial intensity of the emitted light.

[0011] In the above scheme, the control and data processing unit is further used for: An initial co-measurement model is established, wherein the initial co-measurement model includes an absorption coefficient matrix, a concentration matrix, and a transmittance correlation matrix; For each of the multiple solution samples, the transmittance of each rare earth element in the solution sample is input into the transmittance correlation matrix, and the concentration of each rare earth element in the solution sample is input into the concentration matrix. The absorption coefficient matrix of the initial co-measurement model is then solved. Based on the solution of the absorption coefficient matrix, the multi-element co-measurement model is determined.

[0012] In the above scheme, the control and data processing unit is also connected to the X-ray emitter and is also used to adjust the voltage and current parameters of the X-ray emitter.

[0013] This application embodiment also provides a measurement method applied to the control and data processing unit of a measuring device. The measuring device includes an X-ray emitter, a flow cell, and a detector. The X-ray emitter emits X-rays; the flow cell is disposed in the optical path of the X-rays and is used to flow a rare earth solution, the rare earth solution comprising multiple rare earth elements; the detector detects the emitted light after the X-rays irradiate the rare earth solution in the flow cell, generating spectral data of the emitted light. The method includes: Based on the spectral data, the transmittance of each rare earth element in the rare earth solution is determined; The transmittance corresponding to each of the rare earth elements is input into the multi-element simultaneous measurement model to obtain the concentration of each rare earth element in the rare earth solution; wherein, the multi-element simultaneous measurement model is established based on the transmittance and concentration of each rare earth element in multiple solution samples, and the concentration of the various rare earth elements is different in different solution samples.

[0014] The method in the above scheme further includes: The proportions of one or more liquids in the rare earth feed solution, aqueous phase, and organic phase during the rare earth element extraction process are adjusted according to the concentration of each rare earth element in the rare earth solution.

[0015] In the above scheme, determining the transmittance of each rare earth element in the rare earth solution based on the spectral data includes: Based on the spectral data, the absorption edge of each rare earth element among the various rare earth elements is determined; The transmittance of each rare earth element is determined based on its absorption edge.

[0016] In the above scheme, the spectral data represents the radiation intensity corresponding to different energies, and determining the absorption edge of each rare earth element among the multiple rare earth elements based on the spectral data includes: Identify each energy region in which the ray intensity of the spectral data undergoes abrupt changes; The spectral data of each energy region is determined as the absorption edge of the rare earth element.

[0017] In the above scheme, determining the transmittance corresponding to each rare earth element based on its absorption edge includes: Based on the absorption edge of each rare earth element, a first transmittance and a second transmittance of each rare earth element are determined, wherein the first transmittance is the ratio of the first intensity before the change in radiation intensity to the initial intensity of the emitted light, and the second transmittance is the ratio of the second intensity after the change in radiation intensity to the initial intensity of the emitted light.

[0018] The method in the above scheme further includes: An initial co-measurement model is established, wherein the initial co-measurement model includes an absorption coefficient matrix, a concentration matrix, and a transmittance correlation matrix; For each of the multiple solution samples, the transmittance of each rare earth element in the solution sample is input into the transmittance correlation matrix, and the concentration of each rare earth element in the solution sample is input into the concentration matrix. The absorption coefficient matrix of the initial co-measurement model is then solved. Based on the solution of the absorption coefficient matrix, the multi-element co-measurement model is determined.

[0019] The above scheme further includes adjusting the voltage and current parameters of the X-ray emitter.

[0020] The measuring device and method provided in this application enable online measurement of rare earth elements. The device irradiates the rare earth solution to be measured with X-rays and collects the emitted light after irradiation using a detector, obtaining spectral data of the emitted light. This spectral data reflects the transmission characteristics of the rare earth solution. Based on this spectral data, the transmittance of each rare earth element in the solution is determined. Since different rare earth elements have different transmission characteristics, the content of each rare earth element in the solution can be analyzed using its corresponding transmittance. Accordingly, after determining the transmittance of each rare earth element, the transmittances of various rare earth elements are input into a multi-element simultaneous measurement model. The concentration of each rare earth element in the solution is obtained using the multi-element simultaneous measurement model, thereby achieving real-time online continuous measurement of the content of various rare earth elements in the solution. This eliminates the need for manual sampling during extraction and the lengthy sample testing process, saving manpower and material resources. Meanwhile, online measurement results can meet the real-time control requirements of the extraction process, improve the intelligence and automation level of rare earth element extraction, and improve the extraction quality of rare earth elements. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the structure of a measuring device provided in an embodiment of this application; Figure 2 This is a schematic diagram of the absorption spectrum of lanthanum provided in an embodiment of this application; Figure 3This is a schematic flowchart of a measurement method provided in an embodiment of this application; Figure 4 This is a schematic diagram of an absorption spectrum of multiple rare earth elements provided in an embodiment of this application; Figure 5 This is a schematic diagram of a measurement scheme provided in an embodiment of this application. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages of this application clearer, the application will now be described in further detail with reference to the accompanying drawings.

[0023] Rare earth elements include seventeen metallic elements such as lanthanum (La), cerium (Ce), praseodymium (Pr), and neodymium (Nd). Due to their unique optical, electrical, magnetic, and catalytic properties, rare earth elements are widely used in key fields such as new energy materials, high-end equipment manufacturing, metallurgy and chemical industry, and aerospace, and are a strategic key resource for the country.

[0024] In the extraction and separation process of rare earth elements, the rare earth feed solution is typically subjected to multi-stage contact with aqueous and organic phases to achieve the gradual separation and purification of rare earth elements. To ensure the extraction accuracy and purity of rare earth elements, it is necessary to determine the content of various rare earth elements in each stage of the rare earth solution in real time, and then adjust key process parameters such as the number of extraction stages and fluid flow rate based on the content of rare earth elements.

[0025] Currently, in the extraction and separation of rare earth elements, the detection of rare earth elements still heavily relies on offline analysis methods. The adjustment and control of key process parameters in the rare earth element extraction process are all based on the results of offline analysis. This offline analysis method relies on manual sampling, sending the samples to detection equipment for quantitative detection of rare earth elements. After determining the content of various rare earth elements in the sample, the proportions of the aqueous phase, organic phase, and rare earth feed solution during the extraction process are determined manually based on experience, thus achieving the adjustment of the proportions of various liquids. Therefore, this offline analysis method is a form of manual intervention in extraction control.

[0026] The extraction control method based on offline analysis has at least the following drawbacks: First, extraction control methods based on offline analysis suffer from significant time lag. Due to the long intervals between manual sampling, it is difficult to provide real-time feedback on the dynamic changes in the concentrations of various elements in the rare earth solution, making it difficult to adjust process parameters in a timely manner. When abnormal fluctuations occur during the extraction process, it is difficult to quickly identify deviations, which can easily lead to problems such as substandard rare earth element extraction purity and decreased raw material recovery rate, resulting in production losses and economic losses.

[0027] Second, extraction control is highly dependent on human experience. Because different operators have different judgment standards and understandings of the process, the adjustment scale of key process parameters in the extraction process is inconsistent, resulting in significant human interference. This makes it difficult to achieve precise control according to optimal process parameters, thus hindering the improvement of extraction and separation quality.

[0028] To improve the extraction and separation quality of rare earth elements, the following optimization schemes are typically adopted in the rare earth element extraction process: Firstly, the segmented separation process is optimized by adding coarse, fine, and concentrating separation stages, and employing a multi-stage, graded separation architecture with three or four outlets to separate the mixed rare earth solution in multiple stages. For example, the light rare earth portion of the Baotou ore is separated first, i.e., LaCe / PrNd separation is performed first to remove most of the LaCe from the raw material, and then Ce / PrNd separation is carried out. In this way, the LaCe content in the separation stage for PrNd product production is significantly reduced, making process parameter control easier and more beneficial to the quality of rare earth products.

[0029] Secondly, redundant extraction stages are added. Based on the theoretical separation stages, multiple extraction tanks and clarification equipment are added to improve the process tolerance through redundant process margins and reserve adjustment space for fluctuations in the extraction process, so as to improve the extraction quality of rare earth elements.

[0030] While the two optimization schemes mentioned above can improve the stability of the extraction process and reduce the risk of substandard rare earth products to some extent, they still have some drawbacks: the measurement of rare earth element content still relies on manual operation, which makes it difficult to meet the needs of real-time control; the consumption of acid, alkali, organic and other extraction solutions as well as water will increase significantly, increasing the total amount of industrial waste liquid and waste residue discharged; at the same time, the equipment cost and production cycle will increase significantly, which is not conducive to the energy-saving and low-cost development of rare earth products.

[0031] Based on this, embodiments of this application provide a measurement scheme that enables online measurement of rare earth elements using a measuring device. This device irradiates the rare earth solution to be measured with X-rays, and a detector collects the emitted light after the X-rays irradiate the solution, obtaining spectral data of the emitted light. This spectral data reflects the transmission characteristics of the rare earth solution. Based on this spectral data, the transmittance of each rare earth element in the solution is determined. Since different rare earth elements have different transmission characteristics, the content of each rare earth element in the solution can be analyzed using the transmittance corresponding to each rare earth element. Accordingly, after determining the transmittance corresponding to each rare earth element, the transmittances of multiple rare earth elements are input into a multi-element simultaneous measurement model. The concentration of each rare earth element in the solution is obtained using the multi-element simultaneous measurement model, thereby achieving real-time online continuous measurement of the content of multiple rare earth elements in the solution. This eliminates the need for manual sampling during the extraction process and the lengthy sample testing procedure, saving manpower and material resources. Meanwhile, online measurement results can meet the real-time control requirements of the extraction process, improve the intelligence and automation level of rare earth element extraction, and improve the extraction quality of rare earth elements.

[0032] Furthermore, the multi-element simultaneous measurement model is derived from the transmittance and concentration of each rare earth element in multiple solution samples, exhibiting strong generalization ability. By determining the content of each rare earth element in a rare earth solution using this model, the simultaneous measurement of multiple rare earth element contents in the solution can be achieved, improving the efficiency of rare earth element content measurement.

[0033] For ease of understanding, the measuring device provided in the embodiments of this application will be introduced first. This measuring device can also be referred to as an online analysis device for the content of constant rare earth elements. For example, as... Figure 1 As shown, the apparatus provided in this application embodiment includes an X-ray emitter, a flow cell, a detector, and a control and data processing unit.

[0034] An X-ray emitter is used to emit X-rays. Exemplarily, the X-ray emitter includes an X-ray tube. The X-ray tube may be made of materials such as a tungsten target, so that the emitted X-rays match the absorption range of rare earth elements; that is, the frequency range of the X-rays includes the absorption energy range of various rare earth elements. For example, if the absorption range of rare earth elements is 38.39 keV to 63.30 keV, the frequency range of the X-rays includes 38.39 keV to 63.30 keV.

[0035] A flow cell, positioned in the X-ray path, is used to flow a rare earth solution. In some implementations, the flow cell needs to be resistant to high-concentration hydrochloric acid corrosion and absorb almost no X-rays; therefore, materials such as polyethylene (PE), polypropylene (PP), and polystyrene (PS) can be selected for the flow cell. X-rays irradiate the rare earth solution in the flow cell, and the optical path of the X-rays is related to the thickness of the flow cell. The flow cell is typically cuboid, in which case the optical path of the X-rays is equal to the inner diameter of the flow cell. Different optical paths result in varying X-ray absorption intensities for rare earth solutions of the same concentration. An excessively long optical path will cause the rare earth solution to absorb X-rays too completely, making it impossible for the detector to detect the emitted light passing through the rare earth solution; an excessively short optical path may result in insignificant changes in the absorption of X-rays by the rare earth solution, which is detrimental to the analysis of rare earth element concentrations. In some implementations, the inner diameter of the flow cell can be set between 6 mm and 12 mm to meet different detection requirements.

[0036] It is understandable that when X-rays emitted by an X-ray emitter irradiate a rare earth solution in a flow cell, some of the X-rays are absorbed by the solution. The frequency range of the absorbed X-rays (corresponding to the characteristic energies of rare earth elements) is related to the type of rare earth element; different types of rare earth elements have different characteristic energies. Correspondingly, the intensity of the absorbed X-rays is related to the concentration of the rare earth elements and the optical path length of the X-rays (i.e., the thickness of the flow cell). Therefore, by collecting the changes in X-rays before and after passing through the rare earth solution using a detector, the types and concentrations of various rare earth elements in the solution can be analyzed.

[0037] Rare earth solutions include various rare earth elements. For example, rare earth solutions may include lanthanum, cerium, praseodymium, neodymium, and other rare earth elements. A rare earth solution can be a rare earth feed solution or a mixture of a rare earth feed solution and an extraction solution. For example, a rare earth solution can be a mixture of a rare earth feed solution and various extraction solutions such as an aqueous phase or an organic phase. The aqueous phase refers to a liquid system with water as the main solvent, typically including inorganic salts, acids, alkalis, or other water-soluble substances dissolved in water. The organic phase refers to a liquid system with organic solvents as the main solvent, typically including acidic phosphorus compounds, neutral phosphorus compounds, and other organic solvents.

[0038] A detector is used to detect the X-rays emitted after passing through a rare-earth solution in a flow cell, obtaining spectral data of the emitted light. This spectral data represents the intensity of the X-rays corresponding to different energies. For example, an absorption spectrum formed from the spectral data of lanthanum is used as an example. Figure 2As shown, the horizontal axis of the absorption spectrum represents the number of channels, and the vertical axis represents the number of counts. The number of channels indicates the energy of the X-rays; a higher channel number indicates higher energy. The number of counts represents the intensity of the X-rays; a higher count indicates higher intensity. Since the X-rays detected by the detector are the residual X-rays after absorption by the rare earth solution, the spectral data of the emitted light can reflect the absorption of X-rays by each rare earth element in the solution. Therefore, the absorption of X-rays can determine the type and concentration (i.e., content) of the rare earth elements.

[0039] Since the detector is used to collect X-rays emitted from rare earth solutions, the type of detector is related to the energy range of the received X-rays and the energy resolution. In some implementations, cadmium telluride (CdTe) detectors are used. The detection energy range of CdTe detectors is 5 keV to 100 keV, which matches the absorption energy range of rare earth elements. Therefore, collecting X-rays emitted from rare earth solutions using CdTe detectors can provide accurate spectral data for rare earth element analysis.

[0040] The control and data processing unit, connected to the detector, receives spectral data transmitted by the detector and determines the concentrations of multiple rare earth elements in the rare earth solution based on this spectral data. The control and data processing unit can utilize a multi-element simultaneous measurement model to determine the concentrations of multiple rare earth elements in the rare earth solution. Specifically, the control and data processing unit determines the transmittance of each rare earth element in the rare earth solution based on the corresponding spectral data, inputs the transmittances of each rare earth element into the multi-element simultaneous measurement model, and uses the model to determine the concentration of each rare earth element in the rare earth solution, thereby achieving simultaneous measurement of the concentrations of multiple rare earth elements in the rare earth solution.

[0041] In some implementations, the control and data processing unit is also connected to the X-ray emitter, such as via wired or wireless means, to adjust the voltage and current parameters of the X-ray emitter.

[0042] For example, the control and data processing unit can adjust the voltage and current parameters of the X-ray emitter according to the type of rare earth element to be detected. If the rare earth element to be detected is a light rare earth element such as lanthanum or cerium, the control and data processing unit sends a first control command to the X-ray emitter, instructing it to adjust the voltage and current of the X-ray emitter with relatively small first voltage and current parameters. If the rare earth element to be detected is a heavy rare earth element, the control and data processing unit sends a second control command to the X-ray emitter, instructing it to adjust the voltage and current of the X-ray emitter with relatively large second voltage and current parameters. The first voltage parameter is smaller than the second voltage parameter. In this way, by adjusting the voltage and current of the X-ray emitter, the X-ray energy output by the X-ray emitter can be adapted to the rare earth element to be detected.

[0043] For example, the control and data processing unit can adjust the voltage and current parameters of the X-ray emitter based on the spectral data transmitted by the detector. If the count of the spectral data exceeds a first preset count threshold, it indicates that the X-ray intensity is too high, exceeding the detector's detection limit. In this case, the control and data processing unit sends a control command to the X-ray emitter, instructing it to reduce the voltage and current parameters, thereby decreasing the intensity of the emitted X-rays. If the count of the spectral data is less than a second preset count threshold, it indicates that the X-ray intensity is insufficient, making it difficult to effectively identify the absorption signals of rare earth elements. In this case, the control and data processing unit sends a control command to the X-ray emitter, instructing it to increase the voltage and current parameters, thereby increasing the intensity of the emitted X-rays. Thus, by adjusting the voltage and current of the X-ray emitter, the intensity of the emitted X-rays is kept within a suitable range, improving the accuracy of the spectral data.

[0044] In some implementations, the measuring device also includes a peristaltic pump and a flow path. The peristaltic pump is used to pump the rare earth solution from process pipelines such as extraction tanks in the production line into the measuring device through the flow path. Since the rare earth solution is a high-hydrochloric acid matrix, the peristaltic pump and flow path must be resistant to hydrochloric acid corrosion. Therefore, the peristaltic pump can use polytetrafluoroethylene (PTFE) as its liner, and the flow path can be made of fusible polytetrafluoroethylene (PFA), thereby reducing the possibility of corrosion of the peristaltic pump and flow path by the rare earth solution and improving the stability of rare earth solution delivery.

[0045] In some implementations, the measuring device also includes a filter. The filter is used to filter X-rays emitted by the X-ray emitter that are outside the target energy range. The target energy range includes the characteristic energies of various rare earth elements. That is, the filter is used to filter X-rays in energy ranges unrelated to various rare earth elements, such as filtering X-rays outside the absorption energy range of rare earth elements (an example of the target energy range), thereby filtering out or attenuating X-rays in irrelevant energy ranges and improving the detector's ability to capture X-rays. The filtering effect of the filter is related to the filter's material and thickness. For example, the filter can be made of one or more metallic materials such as gold, silver, copper, zinc, and molybdenum. The filter thickness can be set from 0.01 mm to 0.5 mm to achieve the effect of filtering stray scattered lines from irrelevant energy ranges in the X-rays, thereby reducing measurement noise.

[0046] In some implementations, the measuring device also includes a collimator. The collimator controls the X-rays filtered by the filter before they pass through the flow cell and enter the detector. The collimator has a collimation aperture for X-ray passage, used to constrain the X-ray propagation direction and throughput, ensuring that the X-ray propagation direction matches the detector's incident direction and that the X-ray throughput meets the detector's requirements. The amount of X-rays incident on the detector is related to the size of the collimation aperture. A larger collimation aperture results in a larger X-ray throughput, and consequently, a larger amount of X-rays incident on the detector. Conversely, a smaller collimation aperture results in a smaller X-ray throughput, and consequently, a smaller amount of X-rays incident on the detector. To improve the detector's detection performance and ensure stable X-ray input, the amount of X-rays incident on the detector needs to be within a reasonable range. Therefore, the collimation aperture should also be set to a reasonable size to rationally control the amount of X-rays incident on the detector, ensuring that the amount of X-rays incident on the detector matches the detector's effective detection efficiency range. For example, the diameter of the collimating aperture is 0.1 mm to 1.0 mm to ensure a stable amount of X-rays incident on the detector.

[0047] In some implementations, the collimator can be made of tungsten metal. Because tungsten collimators have excellent X-ray shielding properties, they can further block stray scattered rays remaining after filtering, thus optimizing the stability and accuracy of X-ray detection.

[0048] In some implementations, the measuring device further includes a cooling fan and a housing. The cooling fan, disposed inside the measuring device, is used to dissipate heat from the measuring device. Exemplarily, the cooling fan may be positioned adjacent to the X-ray emitter and detector, respectively, so that the cooling fan can dissipate heat from the X-ray emitter and detector. The housing serves to protect the internal components of the measuring device.

[0049] This application embodiment achieves online measurement of the content of multiple rare earth elements in a rare earth solution using a measuring device, thereby meeting the real-time control requirements of the extraction process, improving the intelligence and automation level of rare earth element extraction, and enhancing the extraction quality of rare earth elements. Based on this measuring device, this application embodiment also provides a measurement method. For example, as... Figure 3 As shown, the method includes the following steps: Step 301: Obtain the spectral data corresponding to the rare earth solution. This spectral data is generated based on the emitted light after the rare earth solution in the flow cell is irradiated by X-rays. Step 302: Based on the spectral data corresponding to the rare earth solution, determine the transmittance of each rare earth element in the rare earth solution; Step 303: Input the transmittance corresponding to each rare earth element into the multi-element simultaneous measurement model to obtain the concentration of each rare earth element in the rare earth solution. The multi-element simultaneous measurement model is established based on the transmittance and concentration of each rare earth element in multiple solution samples. The concentrations of various rare earth elements are different in different solution samples.

[0050] In this embodiment of the application, the control and data processing unit of the measuring device acquires the spectral data corresponding to the rare earth solution from the detector, and determines the types and concentrations of various rare earth elements in the rare earth solution based on the spectral data corresponding to the rare earth solution.

[0051] As mentioned above, the spectral data corresponding to the rare earth solution reflects the transmission characteristics of the rare earth solution. Based on the spectral data of the rare earth solution, the control and data processing unit can determine the transmittance of each rare earth element in the solution.

[0052] In some implementations, the control and data processing unit determines the absorption edge of each element in the rare earth solution based on the spectral data of the rare earth solution. Then, based on the absorption edge of each rare earth element, the transmittance of each rare earth element is determined. By calculating the transmittance through the absorption edge characteristics of each rare earth element, the transmittance of each element can be quickly determined, meeting the real-time requirements of online detection of rare earth element extraction.

[0053] Because different rare earth elements (REEs) possess different characteristic energies, their absorption of X-rays occurs in different energy regions. Under the absorption of X-rays by each REE, the X-ray intensity in the spectral data for each REE exhibits abrupt changes within its characteristic energy range; that is, the X-ray intensity drops sharply. Utilizing the absorption characteristics of REEs, the control and data processing unit can identify each energy region where the X-ray intensity abruptly changes in the spectral data corresponding to the rare earth solution. Each energy region corresponds to the characteristic energy of a specific REE. For any given energy region, the control and data processing unit compares this region with the characteristic energies of various REEs to determine the matching characteristic energies, thereby identifying the category of the REE possessing that characteristic energy.

[0054] After determining the rare earth element category corresponding to each energy region where the radiation intensity abruptly changes, the control and data processing unit then identifies the absorption edge of the corresponding coefficient element from the spectral data of each energy region. For example, the absorption spectrum formed from the spectral data corresponding to the rare earth solution is as follows: Figure 4 As shown in the diagram, the absorption spectrum contains multiple energy regions where the X-ray intensity changes abruptly. Each energy region corresponds to the absorption edge of a rare earth element. In order of increasing energy, the absorption edges corresponding to these energy regions are, in order, the absorption edges of La, Ce, Pr, and Nd.

[0055] In some implementations, the control and data processing unit can determine the transmittance of each rare earth element within its corresponding energy region before and after a sudden change in radiation intensity, based on the radiation intensity on both sides of the absorption edge of each rare earth element. For ease of description, the transmittance before the sudden change in radiation intensity is referred to as the first transmittance, and the transmittance after the sudden change in radiation intensity is referred to as the second transmittance. The radiation intensity before the sudden change is referred to as the first intensity, and the radiation intensity after the sudden change is referred to as the second intensity. The control and data processing unit calculates the ratio between the first intensity and the initial intensity of the emitted light, and determines this ratio as the first transmittance. Correspondingly, the control and data processing unit calculates the ratio between the second intensity and the initial intensity of the emitted light, and determines this ratio as the second transmittance.

[0056] The control and data processing unit can determine the maximum ray intensity on both sides of the absorption edge as the first intensity and the minimum ray intensity as the second intensity. To improve the accuracy of the first and second intensities, in some implementations, the control and data processing unit can determine the average or median value of the ray intensity within a first preset interval containing the maximum ray intensity on both sides of the absorption edge as the first intensity, and the average or median value of the ray intensity within a second preset region containing the minimum ray intensity as the second intensity. The first and second preset intervals can be set according to the actual application scenario. The number of spectral data included in the first and second preset intervals is less than a preset value, that is, the interval lengths of the first and second preset intervals are small. The interval lengths of the first and second preset intervals can be the same or different.

[0057] After determining the first and second transmittance of each rare earth element based on the spectral data of the rare earth solution, the control and data processing unit can input the first and second transmittance of each rare earth element into the pre-trained multi-element simultaneous measurement model, and use the multi-element simultaneous measurement model to determine the concentration of each rare earth element in the rare earth solution.

[0058] It is understandable that when only one rare earth element exists in the rare earth solution, the intensity of X-rays passing through the solution depends only on the concentration of the rare earth element being measured and the optical path length of the X-rays. The degree to which X-rays pass through the rare earth solution is represented by the logarithm of the ratio of the transmittance on both sides of the absorption edge of a single rare earth element. The concentration of the rare earth element can then be calculated using formula (1) (also known as the single-boundary algorithm): Formula (1) in, Indicates the concentration of a single rare earth element; and These represent the transmittance on both sides of the absorption edge of a single rare earth element; The value represents the absorption edge coefficient threshold of a single rare earth element, which can be a fixed value; d represents the optical path length of the X-ray.

[0059] When different rare earth elements coexist in large quantities, the absorption edges of rare earth elements with similar atomic numbers will appear simultaneously, resulting in variations in the absorption intensity relative to a single rare earth element. If a single-boundary algorithm is still used to calculate the concentration of rare earth elements, it will produce significant errors. Therefore, in this embodiment, a multi-element co-measurement model based on a "matrix equation" is constructed with reference to the single-boundary algorithm. Simultaneously, the changes in the absorption edges of multiple rare earth elements (such as lanthanum, cerium, praseodymium, and neodymium) when multiple rare earth elements coexist are considered, thus achieving simultaneous measurement of the concentrations of multiple rare earth elements.

[0060] Multi-element simultaneous determination models are used to determine the concentration of each rare earth element in a variety of rare earth elements. For example, a multi-element simultaneous determination model is a matrix model. The following example uses a multi-element simultaneous determination model to determine the concentrations of four constant rare earth elements: lanthanum, cerium, praseodymium, and neodymium. The multi-element simultaneous determination model can be expressed as formula (2): Formula (2) in, Represents the absorption coefficient matrix. ; This represents the absorption edge coefficient of rare earth element x for rare earth element y, which is related to the contribution of absorption edge abrupt change; x and y are positive integers less than or equal to n, used to represent each rare earth element. Represents the concentration matrix. ; This represents the concentration of rare earth element i, where i is a positive integer less than or equal to n, and n equals 4; This represents the transmittance correlation matrix. ; This represents the transmittance-related parameter for rare earth element m, where m is a positive integer less than or equal to n, and n equals 4. The transmittance-related parameter is related to the transmittance of rare earth element m, for example... , This represents the first transmittance of rare earth element m. The second transmittance of rare earth element m is represented by d, which represents the optical path length of X-rays and is equal to the thickness or inner diameter of the flow cell.

[0061] The control and data processing unit inputs the first and second transmittance of each rare earth element into the transmittance correlation matrix of the multi-element simultaneous measurement model, and uses the multi-element simultaneous measurement model to calculate the concentrations of lanthanum, cerium, praseodymium and neodymium in the rare earth solution.

[0062] After obtaining the concentration of each rare earth element in the rare earth solution, the control and data processing unit can also adjust the proportion of one or more liquids in the rare earth feed solution, aqueous phase, and organic phase during the rare earth element extraction process according to the concentration of each rare earth element in the rare earth solution.

[0063] For example, when the concentration of rare earth elements such as praseodymium and neodymium in the rare earth solution is greater than the first preset concentration, it indicates that the current extraction and separation of rare earth elements is insufficient. In this case, the ratio of rare earth feed solution, aqueous phase and organic phase can be adjusted, such as increasing the proportion of organic phase and decreasing the proportion of rare earth feed solution, so that the rare earth feed solution and organic phase can fully contact each other in the extraction tank and improve the extraction efficiency of rare earth elements.

[0064] In this way, the online analysis device (i.e., measuring device) for the content of constant rare earth elements can detect the concentration of various rare earth elements in real time, providing data support for the adjustment of process parameters. This analytical technology eliminates the need for manual sampling and offline analysis, reducing the impact of human factors on the analytical results and enabling real-time measurement of rare earth element content during the rare earth extraction process. Simultaneously, the measured concentration of rare earth elements allows for dynamic adjustment of the amounts of various liquids, effectively optimizing the consumption of acid, alkali, and organic extractants, reducing industrial waste discharge, improving the economic and environmental benefits of extraction and separation, ensuring stable operation of the extraction and separation process, and enhancing the extraction quality of rare earth elements.

[0065] As described above, the control and data processing unit can use a multi-element simultaneous measurement model to determine the concentration of each rare earth element in a rare earth solution. This multi-element simultaneous measurement model is obtained based on the transmittance and concentration of each rare earth element in multiple solution samples. The following example, using the multi-element simultaneous measurement model to determine the concentrations of lanthanum, cerium, praseodymium, and neodymium in a rare earth solution, exemplifies the training process of the multi-element simultaneous measurement model. The training process of the multi-element simultaneous measurement model is executed by the control and data processing unit or other units of the measuring device, or it can be executed by other devices. In this example, the control and data processing unit is uniformly described as the main entity executing the training process of the multi-element simultaneous measurement model.

[0066] First, an initial co-analysis model is established, comprising an absorption coefficient matrix, a concentration matrix, and a transmittance correlation matrix. Then, for each solution sample from multiple solution samples, the transmittance of each rare earth element in each solution sample is input into the transmittance correlation matrix of the initial co-analysis model, and the concentration of each rare earth element in the solution sample is input into the concentration matrix of the initial co-analysis model. The absorption coefficient matrix of the initial co-analysis model is then solved. Finally, based on the solution results of the absorption coefficient matrix, a multi-element co-analysis model is determined.

[0067] To obtain an accurate multi-element co-assay model, the solution samples used for training the model have different rare earth element concentrations. For example, the solution samples include lanthanum, cerium, praseodymium, and neodymium as constant rare earth elements. The concentrations of lanthanum, cerium, praseodymium, and neodymium in each solution sample are shown in Table 1.

[0068] Table 1. Concentrations of various rare earth elements in multiple solution samples

[0069] In this embodiment, multiple solution samples with different concentration ratios can be prepared using a uniform design method. The concentrations of La, Ce, Pr, and Nd in each solution sample range from 10 g / L to 150 g / L. The measuring device irradiates each solution sample with X-rays and collects the emitted light from the irradiated solution sample using a detector, generating spectral data of the emitted light. Based on the spectral data of each solution sample, the control and data processing unit of the measuring device determines the transmittance of each rare earth element in each solution sample and inputs the transmittance and concentration of each rare earth element into the initial co-measurement model. Under the influence of the transmittance and concentration of each rare earth element, the model parameters (such as the absorption coefficient matrix) of the initial co-measurement model are fitted and iteratively trained, ultimately generating a trained multi-element co-measurement model.

[0070] To verify the accuracy of the multi-element simultaneous measurement model, the established online analysis device for constant rare earth element content was used to conduct actual analysis and measurement verification of the rare earth extraction and separation process points. The measurement results are shown in Table 2. The online measurement results are those measured by the measurement device, while the offline sampling analysis results are those analyzed by manual sampling at the process points.

[0071] Table 2 Comparison of online analysis and measurement results with offline sampling analysis results

[0072] It can be seen that the concentrations of each constant rare earth element obtained by the multi-element simultaneous measurement model are basically consistent with the concentrations obtained by the offline sampling method, indicating that the online analysis and measurement scheme of rare earth element content realized by the multi-element simultaneous measurement model has high accuracy and reliability.

[0073] The solutions provided in the embodiments of this application can be referred to. Figure 5 The solution provided in this application reduces interference caused by overlapping absorption edges of multiple rare earth elements in spectral data by constructing a multi-element simultaneous measurement model. By establishing an online analysis and measurement scheme for the content of rare earth elements such as lanthanum, cerium, praseodymium, and neodymium in rare earth extraction and separation processes, it solves the problems of long sampling and analysis cycles, high manpower and material costs in traditional methods, and enables real-time continuous detection of rare earth solutions in multiple process liquid phases such as feed liquid, aqueous phase, and organic phase.

[0074] Based on the above-described measuring device and method, this application embodiment also provides a control and data processing unit, which is applied in the measuring device. The measuring device includes an X-ray emitter, a flow cell, and a detector. The X-ray emitter is used to emit X-rays. The flow cell is disposed in the optical path of the X-rays and is used to flow a rare earth solution, which includes a variety of rare earth elements. The detector is used to detect the emitted light after the X-rays irradiate the rare earth solution in the flow cell and generate spectral data of the emitted light.

[0075] The control and data processing unit includes: A communication interface is used to exchange information with other devices (such as detectors and X-ray emitters); The processor is connected to the communication interface to enable information interaction with other devices and to execute the methods provided by one or more of the above-mentioned technical solutions when running executable instructions or computer programs. The computer program is stored in the memory.

[0076] Specifically, the processor is used for: Based on the spectral data, the transmittance of each rare earth element in the rare earth solution is determined; The transmittance corresponding to each of the rare earth elements is input into the multi-element simultaneous measurement model to obtain the concentration of each rare earth element in the rare earth solution; wherein, the multi-element simultaneous measurement model is established based on the transmittance and concentration of each rare earth element in multiple solution samples, and the concentration of the various rare earth elements is different in different solution samples.

[0077] In some alternative implementations, the processor is further configured to: Based on the concentration of each rare earth element in the rare earth solution, the proportions of one or more liquids in the rare earth feed solution, aqueous phase, and organic phase during the rare earth element extraction process are adjusted.

[0078] In some alternative implementations, the processor is specifically used for: Based on the spectral data, the absorption edge of each rare earth element among the various rare earth elements is determined; The transmittance of each rare earth element is determined based on its absorption edge.

[0079] In some alternative implementations, the processor is specifically used for: Identify each energy region in which the ray intensity of the spectral data undergoes abrupt changes; The spectral data of each energy region is determined as the absorption edge of the rare earth element.

[0080] In some alternative implementations, the processor is specifically used for: Based on the absorption edge of each rare earth element, a first transmittance and a second transmittance of each rare earth element are determined, wherein the first transmittance is the ratio of the first intensity before the change in radiation intensity to the initial intensity of the emitted light, and the second transmittance is the ratio of the second intensity after the change in radiation intensity to the initial intensity of the emitted light.

[0081] In some alternative implementations, the processor is further configured to: An initial co-measurement model is established, wherein the initial co-measurement model includes an absorption coefficient matrix, a concentration matrix, and a transmittance correlation matrix; For each of the multiple solution samples, the transmittance of each rare earth element in the solution sample is input into the transmittance correlation matrix, and the concentration of each rare earth element in the solution sample is input into the concentration matrix. The absorption coefficient matrix of the initial co-measurement model is then solved. Based on the solution of the absorption coefficient matrix, the multi-element co-measurement model is determined.

[0082] In some alternative implementations, the processor is further configured to: Adjust the voltage and current parameters of the X-ray emitter.

[0083] It should be noted that the specific processing procedure of the processor can be understood by referring to the above method.

[0084] Of course, in practical applications, the various components in the control and data processing unit are coupled together through a bus system. The bus system is used to enable communication between these components. In addition to the data bus, the bus system also includes a power bus, a control bus, and a status signal bus.

[0085] The memory in this application embodiment is used to store various types of data to support the operation of the control and data processing unit. Examples of such data include any computer program used to operate on the control and data processing unit.

[0086] The methods disclosed in the embodiments of this application described above can be applied to the processor, or implemented by the processor. The processor may be an integrated circuit chip with signal processing capabilities.

[0087] In implementation, each step of the above method can be completed by the integrated logic circuits in the processor hardware or by instructions in software form. The processor can be a general-purpose processor, a digital signal processor (DSP), or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components, etc. The processor can implement or execute the methods, steps, and logic block diagrams disclosed in the embodiments of this application. The general-purpose processor can be a microprocessor or any conventional processor. The steps of the methods disclosed in the embodiments of this application can be directly manifested as execution by a hardware decoding processor, or execution by a combination of hardware and software modules in the decoding processor. The software modules can be located in a storage medium, which is located in a memory. The processor reads information from the memory and, in conjunction with its hardware, completes the steps of the aforementioned method.

[0088] In an exemplary embodiment, the control and data processing unit may be implemented by one or more application-specific integrated circuits (ASICs), DSPs, programmable logic devices (PLDs), complex programmable logic devices (CPLDs), field-programmable gate arrays (FPGAs), general-purpose processors, controllers, microcontrollers (MCUs), microprocessors, or other electronic components to perform the aforementioned methods.

[0089] It is understood that the memory in the embodiments of this application can be volatile memory or non-volatile memory, or both. Non-volatile memory can be read-only memory (ROM), programmable read-only memory (PROM), erasable programmable read-only memory (EPROM), electrically erasable programmable read-only memory (EEPROM), ferromagnetic random access memory (FRAM), flash memory, magnetic surface memory, optical disc, or compact disc read-only memory (CD-ROM); magnetic surface memory can be disk storage or magnetic tape storage. Volatile memory can be random access memory (RAM), which is used as an external cache. By way of example, but not limitation, many forms of RAM are available, such as Static Random Access Memory (SRAM), Synchronous Static Random Access Memory (SSRAM), Dynamic Random Access Memory (DRAM), Synchronous Dynamic Random Access Memory (SDRAM), Double Data Rate Synchronous Dynamic Random Access Memory (DDRSDRAM), Enhanced Synchronous Dynamic Random Access Memory (ESDRAM), SyncLink Dynamic Random Access Memory (SLDRAM), and Direct Rambus Random Access Memory (DRRAM).The memories described in the embodiments of this application are intended to include, but are not limited to, these and any other suitable types of memories.

[0090] In an exemplary embodiment, this application also provides a storage medium, namely a computer storage medium, specifically a computer-readable storage medium, such as a memory storing executable instructions or a computer program, which can be executed by a processor of a control and data processing unit to complete the steps described in the foregoing method. The computer-readable storage medium may be a memory such as FRAM, ROM, PROM, EPROM, EEPROM, Flash Memory, magnetic surface memory, optical disc, or CD-ROM.

[0091] In an exemplary embodiment, this application also provides a computer program product, including executable instructions or a computer program, which can be executed by the processor of a control and data processing unit to complete the steps described in the foregoing method.

[0092] It should be noted that terms such as "first" and "second" are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence.

[0093] Furthermore, the technical solutions described in the embodiments of this application can be combined arbitrarily without conflict.

[0094] The above description is merely a preferred embodiment of this application and is not intended to limit the scope of protection of this application.

Claims

1. A measuring device, characterized in that, The measuring device includes an X-ray emitter, a flow cell, a detector, and a control and data processing unit; wherein... The X-ray emitter is used to emit X-rays; The flow cell is disposed in the optical path of the X-ray and is used to flow a rare earth solution, wherein the rare earth solution includes a variety of rare earth elements; The detector is used to detect the emitted light after the X-rays irradiate the rare earth solution in the flow cell, and to generate spectral data of the emitted light. The control and data processing unit is connected to the detector and is used to determine the transmittance of each rare earth element among the multiple rare earth elements based on the spectral data. The transmittance of each rare earth element is input into the multi-element simultaneous measurement model to obtain the concentration of each rare earth element in the rare earth solution. The multi-element simultaneous measurement model is obtained based on the transmittance and concentration of each rare earth element in multiple solution samples, and the concentrations of the multiple rare earth elements are different in different solution samples.

2. The apparatus according to claim 1, characterized in that, The control and data processing unit is further configured to: Based on the concentration of each rare earth element in the rare earth solution, the proportions of one or more liquids in the rare earth feed solution, aqueous phase, and organic phase during the rare earth element extraction process are adjusted.

3. The apparatus according to claim 1, characterized in that, The measuring device further includes: A filter is used to filter out X-rays emitted by the X-ray emitter that are outside the target energy range, wherein the target energy range includes the frequency band where the absorption edges of the various rare earth elements are located; A collimator is used to control the X-rays filtered by the filter to pass through the flow cell and then enter the detector.

4. The apparatus according to claim 1, characterized in that, The control and data processing unit is specifically used for: Based on the spectral data, the absorption edge of each rare earth element among the various rare earth elements is determined; The transmittance of each rare earth element is determined based on its absorption edge.

5. The apparatus according to claim 4, characterized in that, The spectral data represents the radiation intensity corresponding to different energies, and the control and data processing unit is specifically used for: Identify each energy region in which the ray intensity of the spectral data undergoes abrupt changes; The spectral data of each energy region is determined as the absorption edge of the rare earth element.

6. The apparatus according to claim 5, characterized in that, The control and data processing unit is specifically used for: For each rare earth element, a first transmittance and a second transmittance are determined on both sides of the absorption edge of the rare earth element, wherein the first transmittance is the ratio of the first intensity before the change in radiation intensity to the initial intensity of the emitted light, and the second transmittance is the ratio of the second intensity after the change in radiation intensity to the initial intensity of the emitted light.

7. The apparatus according to claim 4, characterized in that, The control and data processing unit is further configured to: An initial co-measurement model is established, wherein the initial co-measurement model includes an absorption coefficient matrix, a concentration matrix, and a transmittance correlation matrix; For each of the multiple solution samples, the transmittance of each rare earth element in the solution sample is input into the transmittance correlation matrix, and the concentration of each rare earth element in the solution sample is input into the concentration matrix. The absorption coefficient matrix of the initial co-measurement model is then solved. Based on the solution of the absorption coefficient matrix, the multi-element co-measurement model is determined.

8. The apparatus according to claim 1, characterized in that, The control and data processing unit is also connected to the X-ray emitter and is used to adjust the voltage and current parameters of the X-ray emitter.

9. A measurement method, characterized in that, A control and data processing unit for a measuring device, the measuring device including an X-ray emitter, a flow cell, and a detector; wherein, the X-ray emitter is used to emit X-rays; the flow cell is disposed in the optical path of the X-rays and is used to flow a rare earth solution, the rare earth solution including multiple rare earth elements; the detector is used to detect the emitted light after the X-rays irradiate the rare earth solution in the flow cell, and generate spectral data of the emitted light; the method includes: Based on the spectral data, the transmittance of each rare earth element in the rare earth solution is determined; The transmittance corresponding to each of the rare earth elements is input into the multi-element simultaneous measurement model to obtain the concentration of each rare earth element in the rare earth solution; wherein, the multi-element simultaneous measurement model is established based on the transmittance and concentration of each rare earth element in multiple solution samples, and the concentration of the various rare earth elements is different in different solution samples.

10. The method according to claim 9, characterized in that, The method further includes: An initial co-measurement model is established, wherein the initial co-measurement model includes an absorption coefficient matrix, a concentration matrix, and a transmittance correlation matrix; For each of the multiple solution samples, the transmittance of each rare earth element in the solution sample is input into the transmittance correlation matrix, and the concentration of each rare earth element in the solution sample is input into the concentration matrix. The absorption coefficient matrix of the initial co-measurement model is then solved. Based on the solution of the absorption coefficient matrix, the multi-element co-measurement model is determined.

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