System for separating and purifying carrier-free lutetium 177
By integrating design and pneumatically controlled separation and purification system, the problems of large size and short component life of carrier-free lutetium-177 separation and purification device have been solved, realizing efficient and automated ytterbium-lutetium separation and purification, reducing preparation costs and radiation risks.
Patent Information
- Application Number
- CN202520607373.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-01
- Publication Date
- 2026-02-24
- Estimated Expiration
- 2035-04-01
AI Technical Summary
Existing carrier-free lutetium-177 separation and purification devices are large in size and occupy a large area. They have a high degree of automation and short service life of components. Furthermore, radiation can affect operators and materials.
An integrated separation and purification system is designed, which includes a mounting frame, salt transfer assembly, valve assembly, separation and purification column, sample injection system, fractionation assembly, waste liquid assembly, and sample container. The system achieves fully automated operation through pneumatic valves and air pressure control. The electronic components of each part are located on the outside of the enclosure, using radiation-resistant materials, and are rationally distributed to reduce the system volume.
This method achieves efficient separation and purification of ytterbium-lutetium mixtures, reduces system volume, improves the radiation resistance and service life of components, avoids radiation exposure for operators, and lowers preparation costs.
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Figure CN223936571U_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of radioisotope separation and purification technology, specifically a system for the separation and purification of carrier-free lutetium-177. Background Technology
[0002] Radiotherapy drugs are medical drugs containing radioactive isotopes. In recent years, with the continuous progress of nuclear medicine research, the development of new radionuclides and radiopharmaceuticals has become more targeted, increasing the possibility of preparation according to user requirements and combining radiopharmaceutical diagnostic and therapeutic protocols. This has greatly promoted the market expansion of radiotherapy drugs.
[0003] Lutetium-177 is a therapeutic radionuclide that has attracted much attention in recent years. It emits beta particles with a maximum energy of 0.42 MeV and an average range of 0.67 mm in tissue, making it ideal for treating small or diffuse tumors, as well as tumors unsuitable for surgical resection. In addition, lutetium-177 also emits gamma rays (208 keV), which can be used in single-photon emission computed tomography (SPECT) to monitor and guide the treatment process. Lutetium-177 has a half-life of 6.7 days, making it highly suitable for radiotherapy. Its relatively short half-life minimizes damage to healthy cells during treatment; its relatively long half-life allows for biolabeling and distribution to hospitals after production.
[0004] In existing technologies, there are methods for preparing lutetium-177 by separating and purifying a mixture of ytterbium and lutetium. The separation and purification steps mainly include ytterbium-lutetium separation, lutetium salt concentration, and ytterbium salt recovery. However, these three process steps in existing technologies are typically carried out in different working devices or apparatuses, and the products are then transferred between these devices using transport structures or devices, resulting in a large overall apparatus for lutetium separation and purification. Furthermore, due to the radioactivity of lutetium-177 itself, the entire separation and purification apparatus often requires isolation equipment; the large size and footprint of the overall apparatus further necessitate even larger isolation equipment, indirectly increasing the preparation cost of lutetium-177. In addition, due to the radioactive nature of the samples being processed, a high degree of automation control is required for the entire process to avoid radiation affecting operators. Radiation can also damage materials, causing functional failure and affecting the service life of components. Utility Model Content
[0005] In view of the problems that existing devices for the separation and purification of carrier-free lutetium-177 are large in size and footprint, require a high degree of automation and have short component lifespan, the purpose of this utility model is to provide a system for the separation and purification of carrier-free lutetium-177.
[0006] The objective of this utility model is achieved through the following technical solution:
[0007] This utility model includes a mounting frame, a salt transfer assembly, a valve assembly, a separation and purification column, a sample injection system, a fractionation assembly, a waste liquid assembly, a sample container, and a finished product container. The salt transfer assembly includes a ytterbium salt transfer column and a lutetium salt transfer column, which are respectively mounted on the front side of the mounting frame, with the separation and purification column located on one side of the salt transfer assembly. The valve assembly and the sample injection system are respectively mounted on the rear side of the mounting frame. The fractionation assembly includes a lutetium fractionation tank and a ytterbium fractionation tank. The lutetium fractionation tank is mounted on the mounting frame or located on one side of the mounting frame, while the ytterbium fractionation tank is located on one side of the mounting frame or mounted on the mounting frame. Above; the waste liquid assembly includes at least one waste liquid tank, which is installed on a mounting frame or located on one side of the mounting frame; the sample tank contains a target material solution to be separated, and the control terminal controls the opening and closing of the valves in the sample injection system and valve assembly to control the flow of the target material solution to be separated to the separation and purification column for the separation of ytterbium ions and lutetium ions. The lutetium fraction containing lutetium ions after separation is collected in the lutetium fraction tank, and the ytterbium fraction containing ytterbium ions after separation is collected in the ytterbium fraction tank. The lutetium fraction in the lutetium fraction tank is introduced into the lutetium-to-salt column for lutetium-to-salt concentration, and the ytterbium fraction in the ytterbium fraction tank is introduced into the ytterbium-to-salt column for ytterbium-to-salt recovery.
[0008] Wherein: the mounting frame includes a frame, mounting plate A, and mounting plate B. The frame is the main body of the mounting frame. A separation and purification column is installed on one side of the frame, and mounting plates A and B, which are arranged front and back, are installed on the other side of the frame. The salt transfer assembly is installed on the outward-facing side of mounting plate A, and the valve assembly and sample injection system are installed on the outward-facing side of mounting plate B. The sample container and the finished product container are respectively arranged between mounting plate A and mounting plate B.
[0009] The bottom of the mounting frame is equipped with a material replacement tray for holding parts.
[0010] The lutetium fraction tank is one or more and is mounted on the top of the mounting frame, while the ytterbium fraction tank is located on one side of the mounting frame.
[0011] The waste liquid assembly includes a first waste liquid tank and a second waste liquid tank. The first waste liquid tank is installed on the top of the mounting frame, and the second waste liquid tank and the ytterbium fraction tank are respectively installed on one side of the mounting frame.
[0012] The ytterbium-rotating salt column can be one or multiple columns arranged side by side, and the lutetium-rotating salt column can be one or multiple columns arranged side by side.
[0013] The injection system includes an injection pump and a six-way injection valve with a metering loop. The six-way injection valve is connected to the sample container, the separation and purification column, the waste liquid container and the mobile phase through pipelines. The injection pump is installed on the pipeline.
[0014] The finished product tank includes a ytterbium finished product tank and a lutetium finished product tank. Carrier-free lutetium-177 obtained by lutetium-to-salt concentration is discharged into the lutetium finished product tank, and the solution recovered by ytterbium-to-salt is discharged into the ytterbium finished product tank.
[0015] The front side of the mounting bracket is equipped with an energy spectrum detection probe.
[0016] The valve assembly consists of pneumatic valves, including multiple three-way valves and multiple one-position multi-way valves located on one side of all three-way valves.
[0017] The advantages and positive effects of this utility model are as follows:
[0018] 1. This utility model controls the sample injection system and valve components via a control terminal, thereby controlling the flow of liquid in the separation and purification system. This allows the separation and purification column in the system to separate the ytterbium-lutetium mixture, obtaining fractions containing ytterbium and lutetium ions. These fractions flow into their respective fraction tanks in the fractionation component. The ytterbium and lutetium ions are then post-processed by the corresponding salt transfer component to obtain the corresponding ytterbium and lutetium salts, thus fulfilling the requirement for lutetium separation and purification in the ytterbium-lutetium mixture. The salt transfer component, valve components, separation and purification column, sample injection system, fractionation component, and waste liquid component are rationally arranged on and near the mounting rack. This centralized and rationally distributed arrangement of the various systems for separating and purifying the ytterbium-lutetium mixture ensures that the system can achieve the function of lutetium separation and purification of the ytterbium-lutetium mixture, while the overall system volume is sufficiently small due to the reasonable and compact spatial arrangement and distribution.
[0019] 2. All valve components in this invention are pneumatic valves, and the flow of liquids within the system is achieved pneumatically. Furthermore, the electronic components of each part are located on the outside of the housing, thus preventing the components inside the housing from being affected by radioactive decay, ensuring the overall stability and reliability of the system. Additionally, the radiation resistance of the components is improved by adjusting the materials, guaranteeing their service life. Therefore, this invention, through pneumatic fully automatic control, eliminates the need for operator intervention in the entire process, avoiding the impact of radiation on operators. Moreover, by adjusting materials, adopting a pneumatic control structure, and placing the electronic components on the outside of the housing for radiation resistance, the radiation resistance and service life of each component within the separation and purification system are greatly improved. Furthermore, the rational distribution and connection of the components reduce the volume of the separation and purification system. Attached Figure Description
[0020] Figure 1 This is one of the three-dimensional structural schematic diagrams of this utility model;
[0021] Figure 2 This is the second three-dimensional structural schematic diagram of the present invention;
[0022] Figure 3 This is a front view of the structure of this utility model;
[0023] Figure 4 This is a rear view of the structure of this utility model;
[0024] Figure 5 This is the left structural view of the present invention;
[0025] Figure 6 for Figure 5 Top view;
[0026] Figure 7 This is a schematic diagram of the structural principle of this utility model;
[0027] Wherein: 1 is reagent tank A, 2 is reagent tank B, 3 is reagent tank C, 5 is pump A, 6 is pump B, 7 is pump C, 10 is mounting bracket, 11 is frame, 12 is mounting plate A, 13 is mounting plate B, 14 is material replacement tray, 20 is salt transfer assembly, 21 is ytterbium salt transfer column, 22 is lutetium salt transfer column, 30 is valve assembly, 31 is a single-position multi-way valve, 311 is a single-position four-way valve, 312 is a single-position six-way valve A, 313 is a single-position six-way valve B, 32 is a three-way valve, 320 is a three-way valve A, 321 is a three-way valve B, 322 is a three-way valve C, 3 23 is three-way valve D, 324 is three-way valve E, 325 is three-way valve F, 326 is three-way valve G, 327 is three-way valve H, 328 is three-way valve I, 329 is three-way valve J, 40 is separation and purification column, 50 is sample injection system, 51 is sample injection pump, 52 is six-way sample injection valve, 53 is quantitative loop, 54 is sample container, 60 is distillation assembly, 61 is lutetium distillation container, 62 is ytterbium distillation container, 63 is ytterbium finished product container, 64 is lutetium finished product container, 70 is waste liquid assembly, 71 is first waste liquid container, 72 is second waste liquid container, and 80 is energy dispersive spectroscopy detection probe. Detailed Implementation
[0028] To facilitate understanding of this utility model, a more complete description will be given below with reference to the accompanying drawings. Several embodiments of this utility model are shown in the drawings. However, this utility model can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that the disclosure of this utility model will be more thorough and complete.
[0029] It should be noted that when a component is said to be "fixed to" another component, it can be directly on the other component or there may be an intervening component. When a component is said to be "connected to" another component, it can be directly connected to the other component or there may be an intervening component. The terms "vertical," "horizontal," "left," "right," and similar expressions used in this document are for illustrative purposes only.
[0030] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.
[0031] like Figures 1-7 As shown, this utility model includes a mounting frame 10, a salt transfer assembly 20, a valve assembly 30, a separation and purification column 40, a sample injection system 50, a fractionation assembly 60, a waste liquid assembly 70, a sample container 54, and a finished product container. The salt transfer assembly 20 includes a ytterbium salt transfer column 21 and a lutetium salt transfer column 22. The ytterbium salt transfer column 21, the lutetium salt transfer column 22, and the separation and purification column 40 are respectively installed on the front side of the mounting frame 10, with the separation and purification column 40 located on one side of the salt transfer assembly 20. The valve assembly 30 and the sample injection system 50 are respectively installed on the rear side of the mounting frame 10. The fractionation assembly 60 includes a lutetium fractionation tank 61 and a ytterbium fractionation tank 62. The lutetium fractionation tank 61 is installed on the mounting frame 10 or located on one side of the mounting frame 10, and the ytterbium fractionation tank 62 is located on the rear side of the mounting frame 10. The sample container 54 contains the target solution to be separated. The control terminal controls the opening and closing of the valves in the sample injection system 50 and valve assembly 30, and controls the flow of the target solution to be separated to the separation and purification column 40 for separation of ytterbium ions and lutetium ions. The lutetium fraction containing lutetium ions after separation is collected in the lutetium fraction tank 61, and the ytterbium fraction containing ytterbium ions after separation is collected in the ytterbium fraction tank 62. The lutetium fraction in the lutetium fraction tank 61 is introduced into the lutetium salt conversion column 22 for lutetium salt conversion concentration, and the ytterbium fraction in the ytterbium fraction tank 62 is introduced into the ytterbium salt conversion column 21 for ytterbium salt recovery.
[0032] Understandably, the flow of liquid in the separation and purification system is controlled by the control terminal, which controls the sample injection system 50 and valve assembly 30, so that the separation and purification column 40 separates the ytterbium-lutetium mixture to obtain a ytterbium fraction containing ytterbium ions and a lutetium fraction containing lutetium ions. These fractions flow into the corresponding fraction tanks in the fractionation assembly 60, and then the corresponding salt transfer assembly 20 is used to post-process the ytterbium ions and lutetium ions to obtain the required ytterbium salt and lutetium salt. This fulfills the requirements for the separation and purification of lutetium in the ytterbium-lutetium mixture and the recovery of the raw material ytterbium. By rationally arranging the salt conversion assembly 20, valve assembly 30, separation and purification column 40, sample injection system 50, distillation assembly 60, and waste liquid assembly 70 on and near the mounting frame 10, the various systems for separating and purifying the ytterbium-lutetium mixture are concentrated and rationally distributed. This allows the system to achieve the function of lutetium separation and purification of the ytterbium-lutetium mixture, while the reasonable and compact spatial arrangement and distribution result in a sufficiently small overall system volume. Furthermore, in practical implementation, all valves in each valve assembly 30 are pneumatic valves, and the flow of liquids within the system is achieved pneumatically. The electronic components of each part are located on the outside of the housing, thus avoiding the impact of radioactive decay on the lifespan of the components and ensuring the overall stability and reliability of the system. Therefore, this invention, through pneumatic fully automatic control, eliminates the need for operator intervention in the entire process, avoiding the impact of radiation on operators. Moreover, by adjusting the materials and adopting a pneumatic control structure, the radiation resistance and service life of each component within the separation and purification system are greatly improved. Finally, the rational distribution and connection of the various components reduce the volume of the separation and purification system. Specifically:
[0033] The mounting frame 10 in this embodiment includes a frame 11, a mounting plate A12, and a mounting plate B13. The frame 11 is the main body of the mounting frame 10. A separation and purification column 40 is installed on one side of the frame 11, and mounting plates A12 and B13, arranged front to back, are installed on the other side of the frame 11. A salt transfer assembly 20 is installed on the outward-facing side of mounting plate A12, and a valve assembly 30 and a sample injection system 50 are installed on the outward-facing side of mounting plate B13. In specific implementation, the space within the frame 11 is reasonably divided and used to house the separation and purification column 40 and mounting plates A12 and B13, respectively. Then, by reasonably adjusting the space on mounting plates A12 and B13, the salt transfer assembly 20, the sample injection system 50, and the valve assembly 30 are respectively used to house the other components. This allows the irregularly shaped components to be reasonably distributed and arranged on the regular frame 11, making reasonable and effective use of space and greatly reducing the overall system footprint. In addition, a sample container 54 and a finished product container are installed between mounting plate A12 and mounting plate B13. The injection system 50 is connected to the sample container 54, the six-way injection valve 52, the injection pump 51, and the feeding equipment via pipelines. Specifically, the six-way injection valve 52 with a quantitative loop 53 is connected to the reagent container C3, the sample container 54, the separation and purification column 40, and the second waste liquid container 72 via pipelines. An injection pump 51 is installed on the pipeline connected to the second waste liquid container 72. Furthermore, in a specific implementation, the finished product containers include a ytterbium finished product container 63 and a lutetium finished product container 64. The carrier-free lutetium-177 obtained by lutetium-to-salt concentration is discharged into the lutetium finished product container 64, and the solution recovered by ytterbium-to-salt is discharged into the ytterbium finished product container 63. By installing the sample container 54 and the finished product container between mounting plate A12 and mounting plate B13, the space within the mounting frame 10 is utilized as much as possible.
[0034] In this embodiment, a material replacement tray 14 is provided at the bottom of the mounting frame 10. The material replacement tray 14 is used to hold replacement parts. Specifically, the material replacement tray 14 can hold salt transfer columns, separation and purification columns 40, valves, etc. These components are replaced, disassembled, and repaired using a robotic arm. As an example, and not a limitation, in some alternative embodiments, the material replacement tray 14 is in the form of a seesaw. The replacement part is placed at one end, and then the robotic arm presses it at the other end, causing the part to move closer to the robotic arm, which then picks it up for replacement.
[0035] In this embodiment, the valve assembly 30 consists of pneumatic valves, including multiple evenly distributed three-way valves 32 and multiple one-position multi-way valves 31 located on one side of all three-way valves 32. In specific implementations, the relative positions of the three-way valves 32 and the one-position multi-way valves 31 can be adjusted according to the specific installation conditions to ensure efficient use of space. By setting multiple different valves, the flow of liquid within the system is controlled to ensure stable and accurate operation of the production process. Specifically, an energy dispersive spectroscopy (EDS) probe 80 is provided on the mounting bracket 10 near the salt transfer assembly 20. The EDS probe 80 is used to monitor the effluent time of each product within the system to assist the operation of the valve assembly 30 and the sample introduction system 50. Furthermore, a temperature sensor is also provided on the separation and purification column 40 to detect the temperature of the separation and purification column 40, ensuring that the separation and purification column 40 operates within the optimized temperature range. Additionally, the installation position of the EDS probe 80 can also be adjusted according to actual conditions to optimize space utilization and is not limited thereto. The three-way valves in this embodiment include a three-way valve A320 located at the input end of the separation and purification column 40, a three-way valve B321 located at the output end of the separation and purification column 40, a three-way valve C322 located at the input end of the ytterbium-to-salt column 21, a three-way valve D323 located at the output end of the ytterbium-to-salt column 21, a three-way valve E324 located at the input end of the lutetium-to-salt column, a three-way valve F325 located at the output end of the lutetium-to-salt column, and a three-way valve G326 located on the pipeline between three-way valve D323 and the ytterbium finished product tank 63. The three-way valves in this embodiment include a three-way valve H327 on the pipeline between the three-way valve 325F and the lutetium product tank 64, a three-way valve I328 connected to the reagent tank A1 via a pipeline, and a three-way valve J329 connected to the reagent tank B2 via a pipeline. The single-position multi-way valves in this embodiment include a single-position four-way valve 311 on the pipeline between the three-way valve B321 and the ytterbium fraction tank 62, a single-position six-way valve A312 at the input end of each lutetium fraction tank 61, and a single-position six-way valve B313 at the output end of each lutetium fraction tank 61.
[0036] In this embodiment, two separation and purification columns 40 are arranged side by side. The input ends of the two separation and purification columns 40 are equipped with three-way valves A320. The first port of three-way valve A320 is connected to a six-way injection valve 52 via a pipeline, and the second and third ports are respectively connected to the input ends of the two separation and purification columns 40. The output ends of the two separation and purification columns 40 are equipped with three-way valves B321. The first port of three-way valve B321 connects to the ytterbium fractionation tank 62 via an energy dispersive spectroscopy probe 80 and a one-position four-way valve 311. The second and third ports of three-way valve B321 are respectively connected to the output ends of the two separation and purification columns 40. The other two ports of the one-position four-way valve 311 are respectively connected to a second waste liquid tank 72 and the input end of a one-position six-way valve A312 via pipelines. The packing material in the separation and purification columns 40 of this embodiment can be the packing material prepared in Example 1 of CN102614845A, published on August 1, 2012.
[0037] This embodiment includes five lutetium fractionation tanks 61 and one ytterbium fractionation tank 62. The five lutetium fractionation tanks 61 are all located on top of the mounting frame 10, and the one ytterbium fractionation tank 62 is located on one side of the mounting frame 10. In practice, the amount of ytterbium-lutetium mixture to be separated and purified each time is determined by introducing the ytterbium-lutetium mixture from the sample tank 54 into the quantitative loop 53. By setting up five lutetium fractionation tanks 61, when the ytterbium-lutetium mixture in one sample tank 54 is sequentially introduced into the quantitative loop 53 for multiple separations and purifications, the lutetium ions separated each time can be stored separately, ensuring the independence of each separation and purification, thus preventing errors and avoiding mutual interference between different rounds of separation. The input ends of the five lutetium fractionation tanks 61 and the first waste liquid tank 71 are equipped with a one-position six-way valve A312. The input ends of the one-position six-way valve A312 are connected to the reagent tank A1 and the one-position four-way valve 311 respectively through pipelines. The output ends of the five lutetium fractionation tanks 61 and the first waste liquid tank 71 are equipped with a one-position six-way valve B313. The output end of the one-position six-way valve B313 is connected to the lutetium salt column 22 through pipelines.
[0038] The waste liquid assembly 70 in this embodiment includes a first waste liquid tank 71 and a second waste liquid tank 72. The first waste liquid tank 71 is located on the top of the mounting frame 10 near the ytterbium fraction tank 62. The second waste liquid tank 72 and the ytterbium fraction tank 62 are respectively located on one side of the mounting frame 10. The second waste liquid tank 72 is used to collect wastewater during separation and during the overall cleaning of the system before and after separation. Therefore, the wastewater volume is relatively large, and consequently, the second waste liquid tank 72 is also relatively large, hence its separate installation. The first waste liquid tank 71 is used for waste liquid collection during the lutetium-to-salt conversion process. Alternatively, the second waste liquid tank 72 can be used for waste liquid collection during the ytterbium-to-salt conversion process, and the first waste liquid tank 71 can be used for waste liquid collection during the lutetium-to-salt conversion process, or both the second waste liquid tank 72 and the first waste liquid tank 71 can be used for waste liquid collection during the ytterbium-to-salt conversion process, or both can be used for waste liquid collection during the lutetium-to-salt conversion process. Because the amount of waste liquid generated during the lutetium-to-salt conversion process is small, the first waste liquid tank 71 is small in size and is located on the top of the mounting frame 10, near the ytterbium fraction tank 62. Furthermore, based on their size, the two waste liquid tanks are rationally positioned to reduce the overall system footprint. In addition, in practical implementation, the first waste liquid tank 71 and the second waste liquid tank 72 can be interchanged by adjusting the pipeline connections and valve controls, and are not limited to collecting any particular type of waste liquid.
[0039] In this embodiment, two ytterbium transfer columns 21 and two lutetium transfer columns 22 are arranged side by side. Two transfer columns are installed for each of the ytterbium and lutetium transfer columns, ensuring that if one transfer column is damaged or needs cleaning, a spare transfer column is available, guaranteeing stable operation of the production process. The ytterbium transfer column 21 in this embodiment (a PEEK column with an inner diameter of 20 mm and a length of 150 mm) is packed with a strong cation exchange resin (…). 50WX8 cation exchange resin), lutetium-modified salt column 22 (PEEK column with inner diameter of 4.6 mm and length of 100 mm) packed with strong cation exchange resin ( 50WX8 cation exchange resin).
[0040] In this embodiment, reagent tanks A1, B2, and C3 are respectively provided, and pumps A5, B6, and C7 are respectively installed on the outlet pipes of reagent tanks A1, B2, and C3.
[0041] As an example, and not a limitation, in some alternative embodiments, the specific usage of this utility model is as follows:
[0042] First, the mobile phase (such as eluent or rinsing agent) in reagent tank C3 is controlled by the injection system 50 to flush the entire system at a preset flow rate. The flow path is as follows: the feeding equipment delivers the mobile phase, which enters any separation and purification column 40 through the injection system 50 via the six-way injection valve 52 and the three-way valve A320. After flowing out through the three-way valve B321 and being detected by the energy dispersive spectroscopy probe 80, it is discharged into the second waste liquid tank 72 through the one-position four-way valve 311.
[0043] The control terminal switches the six-way injection valve 52, drawing the ytterbium-lutetium mixture in the sample container 54 into the quantitative loop 53. Then, the six-way injection valve 52 is switched again, and the injection pump 51 draws in the mobile phase from the reagent container C3. The sample is then carried into the separation and purification column 40 by the mobile phase, and the separation process officially begins. The final destination depends on the signal from the energy dispersive spectroscopy (EDS) detection probe 80. Based on the signal provided by the EDS detection probe 80, the switching of the one-position four-way valve 311 is controlled. When a lutetium signal is detected, the sample flows through the one-position six-way valve A312 to the lutetium fraction tank 61 (due to space constraints in the hot chamber, this embodiment can perform a maximum of five separations; to prevent errors, the lutetium fraction is collected separately each time, hence five lutetium fraction tanks 61 are provided. The number of lutetium fraction tanks does not affect the implementation of this separation process); when a ytterbium signal is detected, the sample flows to the ytterbium fraction tank 62; otherwise, the sample flows to the second waste tank 72. After separation, the separation and purification column 40 can be washed and stored with 10% to 100% methanol; otherwise, it can be left unsold, depending on the characteristics of the separation and purification column 40.
[0044] The separated lutetium fraction contains organic acid eluent, which does not meet the requirements for final use. Therefore, a salt-concentration step is needed. This step not only removes the eluent and converts it into a medical-grade lutetium chloride solution, but also concentrates the lutetium product (the separated lutetium fraction is very dilute). Specifically:
[0045] System replacement: Water from reagent tank B2 is used to replace the storage solution in the system via a feeding device. The water flows through three-way valve J329, three-way valve E324, lutetium-to-salt column 22, three-way valve F325, three-way valve H327, and one-position six-way valve A312 before being discharged into the first waste liquid tank 71. Sample preparation: 2M hydrochloric acid from reagent tank A1 is sequentially pumped into the lutetium fraction tank 61 containing lutetium fraction via one-position six-way valve A312. The liquid is then uniformly mixed by gas stirring. Sample loading: The liquid from the lutetium fraction tank 61 is sequentially loaded into the lutetium-to-salt column 22 via one-position six-way valve B313 and three-way valve E324. Luteinium ions are adsorbed in the lutetium-to-salt column 22. If a pump is used for sample loading, radiation will damage the pump's circuit board, causing system failure. Considering radiation protection, this system selects to load samples via gas pressure, or liquid transfer can be performed using a pump; rinsing: water from reagent tank B2 is passed through three-way valves J329 and E324 to the lutetium-to-salt column 22 to remove residual organic acid eluent. The waste liquid is discharged into the first waste liquid tank 71 through three-way valves F325, H327, and a single-position six-way valve A312; elution: the reagent tank... A1 is manually replaced with 0.15mM hydrochloric acid. The 0.15mM hydrochloric acid is pumped into the lutetium-to-salt column 22 via three-way valves I328 and E324 using pump A5. The 0.15mM hydrochloric acid washes away the lutetium ions adsorbed in the lutetium-to-salt column 22, resulting in a concentrated lutetium chloride solution. This solution is then collected in the lutetium finished product tank 64 via three-way valves F325 and H327. After the lutetium-to-salt concentration is completed, the product can be transferred to the required location. The lutetium-to-salt column 22 can be regenerated and stored as needed.
[0046] The separated ytterbium fraction contains organic acid eluent, which is detrimental to precipitation recovery. Therefore, a salt-concentration step is required. This step removes the eluent and converts the ytterbium into a ytterbium chloride solution, facilitating further precipitation and calcination to ytterbium oxide (for recycling as a target material). Specifically:
[0047] System replacement: The water in reagent tank B2 replaces the storage solution in the system through the feeding device. The solution flows through three-way valve J329, three-way valve C322, ytterbium-to-salt column 21, three-way valve D323, and three-way valve G326 before being discharged into the second waste tank 72. Sample preparation: 2M hydrochloric acid from reagent tank A1 is pumped through pump A5 into the ytterbium fraction tank 62 containing the ytterbium fraction. The liquid is then uniformly mixed using gas stirring. Sample loading: The liquid from the ytterbium fraction tank 62 is loaded into the ytterbium-to-salt column 21 through three-way valves J329 and C322, allowing ytterbium ions to be adsorbed onto the column. Washing: Using reagent tank B2... Water flows through three-way valves J329 and C322 into the ytterbium-converted salt column 21 to remove residual organic acid eluent. The waste liquid is discharged into the second waste liquid tank 72 through three-way valves D323 and G326. Elution: The reagent tank A1 is manually replaced with 0.15mM hydrochloric acid. The 0.15mM hydrochloric acid is pumped into the ytterbium-converted salt column 21 through three-way valves I328 and C322 via pump A5. The ytterbium ions adsorbed in the ytterbium-converted salt column 21 are washed off by the 0.15mM hydrochloric acid, and a high-purity ytterbium chloride solution is obtained. After passing through three-way valves D323 and G326, the solution is collected in the ytterbium finished product tank 63. After the ytterbium-converted salt recovery is completed, the product is transferred to the required location and then the precipitation and calcination processes are continued to obtain ytterbium oxide powder. The ytterbium-converted salt column 21 is regenerated and preserved as needed.
[0048] Additionally, the control terminal includes at least a processor and a memory. In some embodiments, the processor may be a Central Processing Unit (CPU), a controller, a microcontroller, a microprocessor, or other data processing chip, used to run program code stored in the memory or process data, such as executing access restriction programs. The memory includes at least one type of readable storage medium, including flash memory, hard disk, multimedia card, card-type memory (e.g., SD or DX memory), magnetic memory, magnetic disk, optical disk, etc. In some embodiments, the memory may be an internal storage unit of the electronic device, such as the hard disk of the electronic device. In other embodiments, the memory may be an external storage device of the electronic device, such as a plug-in hard disk, SmartMedia Card (SMC), Secure Digital (SD) card, Flash Card, etc. Furthermore, the memory may include both internal storage units and external storage devices of the electronic device. The memory can be used not only to store application software and various types of data of the electronic device, but also to temporarily store data that has been output or will be output.
[0049] Furthermore, the system of this invention also includes a sealing element used for sealing the components within the system. The sealing element is made of a radiation-resistant material. By way of example, and not limitation, in some optional embodiments, sealing elements are typically provided at the connections or on pneumatic valves of the system. By using a radiation-resistant material for the sealing element, the lifespan of the component can be effectively extended. It should be noted that, as can be seen from the above system usage flow, this invention achieves fully automated separation and purification of ytterbium-lutetium mixtures by rationally and automatically controlling the opening and closing of valves and the flow of liquid. This allows the system to operate fully automatically, avoiding radiation exposure for workers and improving production efficiency. In addition, the system of this invention adopts an integrated design, enabling automated operation within a smaller space, reducing the cost of large-scale automated control, and allowing the automated control of this invention to conform to actual production cost conditions. In addition, to avoid the impact of radiation on the system's lifespan, the design and manufacturing of this invention fully consider radiation resistance. For example, the sealing ring has been changed from ordinary polytetrafluoroethylene rubber to EPDM rubber, the electronic control mechanism in the system has been replaced with a pneumatic control mechanism, and the liquid transfer inside the hot chamber is controlled by air pressure.
[0050] In summary, the separation and purification system described in the above embodiments of this utility model controls the sample injection system 50 and valve assembly 30 via a control terminal to control the flow of liquid in the separation and purification system. This allows the separation and purification column 40 to separate the ytterbium-lutetium mixture, obtaining fractions containing ytterbium ions and lutetium ions, which then flow into the corresponding fraction tanks within the fractionation assembly 60. The ytterbium ions and lutetium ions are then post-processed by the corresponding salt transfer assembly 20 to obtain the desired ytterbium salt and lutetium salt, thus fulfilling the requirements for the separation and purification of lutetium in the ytterbium-lutetium mixture and the recovery of the raw material ytterbium. By rationally arranging the salt conversion assembly 20, valve assembly 30, separation and purification column 40, sample injection system 50, distillation assembly 60, and waste liquid assembly 70 on and near the mounting frame 10, the various systems for separating and purifying the ytterbium-lutetium mixture are concentrated and rationally distributed. This allows the system to achieve the function of lutetium separation and purification of the ytterbium-lutetium mixture, while the reasonable and compact spatial arrangement and distribution result in a sufficiently small overall system volume. Furthermore, in practical implementation, all valves in each valve assembly 30 are pneumatic valves, and the flow of each liquid within the system is achieved pneumatically. Therefore, this invention, through pneumatic fully automatic control, eliminates the need for operator intervention in the entire process, avoiding the impact of radiation on operators. Moreover, by adjusting the materials and adopting a pneumatic control structure, the radiation resistance and service life of each component within the separation and purification system are greatly improved. Finally, the rational distribution and connection of the various components reduce the volume of the separation and purification system.
[0051] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0052] The embodiments described above are merely illustrative of several implementations of this utility model, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of this utility model patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this utility model, and these all fall within the protection scope of this utility model. Therefore, the protection scope of this utility model patent should be determined by the appended claims.
Claims
1. A system for the separation and purification of carrier-free lutetium-177, characterized in that: The system includes a mounting frame (10), a salt transfer assembly (20), a valve assembly (30), a separation and purification column (40), a sample injection system (50), a fractionation assembly (60), a waste liquid assembly (70), a sample container (54), and a finished product container. The salt transfer assembly (20) includes a ytterbium salt transfer column (21) and a lutetium salt transfer column (22), which are respectively mounted on the front side of the mounting frame (10). The separation and purification column (40) is located on one side of the salt transfer assembly (20). The valve assembly (30) and the sample injection system (50) are respectively mounted on the rear side of the mounting frame (10). The fractionation assembly (60) includes a lutetium fractionation tank (61) and a ytterbium fractionation tank (62), which are mounted on the mounting frame (10) or located on one side of the mounting frame (10). The sub-tank (62) is located on one side of the mounting frame (10) or mounted on the mounting frame (10); the waste liquid assembly (70) includes at least one waste liquid tank, which is mounted on the mounting frame (10) or located on one side of the mounting frame (10); the sample tank (54) contains the target material solution to be separated, and the control terminal controls the opening and closing of the valves in the sample injection system (50) and valve assembly (30) to control the target material solution to be separated. The liquid flows to the separation and purification column (40) for the separation of ytterbium ions and lutetium ions. The lutetium fraction containing lutetium ions after separation is collected in the lutetium fraction tank (61), and the ytterbium fraction containing ytterbium ions after separation is collected in the ytterbium fraction tank (62). The lutetium fraction in the lutetium fraction tank (61) is introduced into the lutetium salt conversion column (22) for lutetium salt concentration. The ytterbium fraction in the ytterbium fraction tank (62) is introduced into the ytterbium salt conversion column (21) for ytterbium salt recovery.
2. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The mounting frame (10) includes a frame (11), mounting plate A (12), and mounting plate B (13). The frame (11) is the main body of the mounting frame (10). A separation and purification column (40) is installed on one side of the frame (11), and mounting plates A (12) and B (13) are installed on the other side of the frame (11). The salt transfer assembly (20) is installed on the side of mounting plate A (12) facing outwards, and the valve assembly (30) and the injection system (50) are installed on the side of mounting plate B (13) facing outwards. The sample container (54) and the finished product container are respectively arranged between mounting plate A (12) and mounting plate B (13).
3. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The bottom of the mounting bracket (10) is provided with a material replacement tray (14) for holding parts.
4. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The lutetium fraction tank (61) is one or more and is mounted on the top of the mounting frame (10), and the ytterbium fraction tank (62) is located on one side of the mounting frame (10).
5. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The waste liquid assembly (70) includes a first waste liquid tank (71) and a second waste liquid tank (72). The first waste liquid tank (71) is installed on the top of the mounting frame (10), and the second waste liquid tank (72) and the ytterbium fraction tank (62) are respectively arranged on one side of the mounting frame (10).
6. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The ytterbium-rotating salt column (21) can be one or multiple columns arranged side by side, and the lutetium-rotating salt column (22) can be one or multiple columns arranged side by side.
7. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The injection system (50) includes an injection pump (51) and a six-way injection valve (52) with a metering loop (53). The six-way injection valve (52) is connected to the sample container (54), the separation and purification column (40), the waste liquid container and the mobile phase through pipelines. The injection pump (51) is installed on the pipeline.
8. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The finished product tanks include a ytterbium finished product tank (63) and a lutetium finished product tank (64). The carrier-free lutetium-177 obtained by lutetium-to-salt concentration is discharged into the lutetium finished product tank (64), and the solution recovered by ytterbium-to-salt is discharged into the ytterbium finished product tank (63).
9. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The mounting bracket (10) is equipped with an energy spectrum detection probe (80) on its front side.
10. The system for carrier-free lutetium-177 separation and purification according to claim 1, characterized in that: The valve assembly (30) consists of pneumatic valves, including multiple three-way valves (32) and multiple one-position multi-way valves (31) disposed on one side of all three-way valves (32).
Citation Information
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Strong cation exchange chromatographic stationary phase and preparation method thereof
CN102614845A