Device for separating and purifying carrier-free lutetium 177
By designing an integrated lete-177 separation and purification device, the arrangement of the mounting frame and the control of pneumatic valves are used to solve the problems of large device size, high automation control and short parts life in the prior art, and efficient lete-treateri separation and purification and improvement of radiation resistance are achieved.
Patent Information
- Application Number
- CN202510402480.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-01
- Publication Date
- 2025-05-02
- Estimated Expiration
- 2045-04-01
AI Technical Summary
In the prior art, the overall separation and purification device without carrier lete-177 has a large volume, a large area of land, a high degree of automation control and a short service life of parts.
An integrated separation and purification device is designed, and the salt transfer assembly, valve assembly, separation and purification column, injection system, fraction assembly and waste liquid assembly are reasonably arranged through the mounting frame. The pneumatic valve and pneumatic pressure fully automatic control are adopted to reduce the device volume and improve the radiation resistance of parts.
It realizes efficient separation and purification of bblt-drug mixture, reduces the device volume and footprint, improves the automation control level and the service life of parts, and avoids the impact of radiation on operators and materials.
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Figure CN119913379A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of separation and purification of radioactive isotopes, in particular to a device for separation and purification of carrier-free lutetium-177. Background Art
[0002] Radioactive therapeutic drugs are medical drugs containing radioactive isotopes. In recent years, with the continuous progress of nuclear medicine research, the development of new radionuclides and radioactive drugs has greater targeting, increasing the possibility of preparing according to user requirements and combining radioactive drug diagnosis and treatment programs, which has greatly promoted the market expansion of radioactive therapeutic drugs.
[0003] Lutetium-177 is a therapeutic radionuclide that has attracted much attention in recent years. The maximum energy of the beta particles it emits is 0.42 MeV, and the average range in the tissue is 0.67 mm, which is very suitable for treating small or diffuse tumors, as well as tumors that are not suitable for surgical resection. In addition, Lutetium-177 also emits gamma rays (208 keV) and can be used for single-photon emission computed tomography (SPECT) to monitor and guide the treatment process. The half-life of Lutetium-177 is 6.7 days, making it very suitable for radiotherapy. The relatively short half-life minimizes damage to healthy human cells during the entire treatment; its relatively long half-life allows it to be labeled with biological molecules and delivered to hospitals after production.
[0004] In the prior art, there is a method of preparing lutetium-177 by separation and purification from a mixture of ytterbium and lutetium, wherein the steps of separation and purification mainly include ytterbium and lutetium separation, lutetium transsalt concentration and ytterbium transsalt recovery. In the prior art, these three process steps are usually carried out in different working equipment or devices, and then each product is transported between different devices through a transport structure or device, which makes the overall device for separation and purification of lutetium bulky. And due to the radioactivity of lutetium-177 itself, most of the overall devices for separation and purification need to be isolated with isolation equipment; and the overall device for separation and purification has a large volume and floor space, which also requires larger isolation equipment, which increases the preparation cost of lutetium-177 in disguise. In addition, due to the radiation properties of the processed samples, the degree of automation control of the entire process step is very high to avoid the impact of radiation on the operator. Radiation can also damage materials, cause functional failures, and affect the service life of parts. Summary of the invention
[0005] In view of the problems in the prior art that the overall device for separation and purification of carrier-free lutetium-177 is large in size and occupies a large area, requires a high degree of automation control and has a short service life of components, the object of the present invention is to provide a device for separation and purification of carrier-free lutetium-177.
[0006] The objective of the present invention is achieved through the following technical solutions: The invention comprises a mounting frame, a salt conversion assembly, a valve assembly, a separation and purification column, a sampling system, a fraction assembly, a waste liquid assembly, a sample tank and a finished product tank, wherein the salt conversion assembly comprises an ytterbium salt conversion column and a lutetium salt conversion column, the ytterbium salt conversion column, the lutetium salt conversion column and the separation and purification column are respectively mounted on the front side of the mounting frame, and the separation and purification column is located on one side of the salt conversion assembly; the liquid inlet and outlet ends of the ytterbium salt conversion column and the lutetium salt conversion column are both provided with quick-connect joints, and the mounting frame above the ytterbium salt conversion column and the lutetium salt conversion column is provided with a quick-connect joint. The mounting frame below the ytterbium-converted salt column and the lutetium-converted salt column is fixed with cylinders of equal number and one-to-one correspondence to the quick-connect joints at each liquid outlet end, and the cylinders control the corresponding quick-connect joint switches to achieve the connection or disconnection between the ytterbium-converted salt column and the lutetium-converted salt column and the pipeline; the valve assembly and the injection system are respectively mounted on the rear side of the mounting frame; the fraction assembly includes a lutetium fraction tank and a ytterbium fraction tank, the lutetium fraction tank is mounted on the mounting frame or on one side of the mounting frame, and the ytterbium fraction tank is arranged on one side of the mounting frame or on the mounting frame; the waste liquid assembly includes at least one waste liquid tank, which is mounted on the mounting frame or on one side of the mounting frame; an energy spectrum detection probe is arranged on the front side of the mounting frame, an ultraviolet detector is arranged on the mounting frame below the valve assembly, and an ultraviolet detector and a reaction tube are respectively arranged on the pipeline between the separation and purification column and the waste liquid tank; the sample tank The target material solution to be separated is contained therein, and the control terminal controls the on-off of the valve in the sampling system and the valve assembly, controls the target material solution to be separated to flow to the separation and purification column to separate ytterbium ions and lutetium ions, collects the lutetium fraction containing lutetium ions after separation in the lutetium fraction tank, collects the ytterbium fraction containing ytterbium ions after separation in the ytterbium fraction tank, introduces the lutetium fraction in the lutetium fraction tank into the lutetium conversion salt column for lutetium conversion salt concentration, and introduces the ytterbium fraction in the ytterbium fraction tank into the ytterbium conversion salt column for ytterbium conversion salt recovery.
[0007] Wherein: the mounting frame includes a frame, a mounting plate A, and a 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 a mounting plate A and a mounting plate B arranged in front and behind are installed on the other side of the frame, the salt transfer assembly is installed on the outward side of the mounting plate A, and the valve assembly and the injection system are installed on the outward side of the mounting plate B; the sample tank and the finished product tank are respectively arranged between the mounting plate A and the mounting plate B.
[0008] A material replacement tray for holding parts is provided at the bottom of the mounting frame.
[0009] The lutetium fraction tank is one or more and is installed on the top of the mounting frame, and the ytterbium fraction tank is arranged on one side of the mounting frame.
[0010] The waste liquid assembly includes a first waste liquid tank, a second waste liquid tank and a third waste liquid tank. The first waste liquid tank is installed on the top of the mounting frame, the second waste liquid tank and the third waste liquid tank are respectively arranged on one side of the mounting frame, and the ytterbium fraction tank is arranged on the top of the second waste liquid tank.
[0011] The ytterbium-converted salt column is one or a plurality of columns arranged side by side, and the lutetium-converted salt column is one or a plurality of columns arranged side by side.
[0012] The injection system comprises an injection pump and a six-way injection valve with a quantitative loop. The six-way injection valve is connected to a sample tank, a separation and purification column, a waste liquid tank and a mobile phase through pipelines respectively, and the injection pump is arranged on the pipeline.
[0013] The finished product tank includes an ytterbium finished product tank and a lutetium finished product tank. The carrier-free lutetium-177 obtained by lutetium transsalting and concentration is discharged into the lutetium finished product tank, and the solution recovered by ytterbium transsalting is discharged into the ytterbium finished product tank.
[0014] The device is cleaned before separation and purification, and the mobile phase transported by the feeding equipment enters the device after being heated by the heat exchanger; the heat exchanger includes a shell, a heating rod, a temperature sensor A, a coil rack and a heat exchange coil, the shell is filled with a heat-conducting medium, the top of the shell is respectively provided with a liquid inlet A and a liquid outlet, a coil rack is installed inside the shell, a heat exchange coil is wound on the coil rack, and the two ends of the heat exchange coil are respectively connected with the liquid inlet A and the liquid outlet; a heating rod and a temperature sensor A are respectively arranged inside the coil rack, the heating rod, the temperature sensor A, the coil rack and the heat exchange coil are all immersed in the heat-conducting medium, the upper ends of the heating rod and the temperature sensor A are fixed on the shell, the heating rod is energized to heat the heat-conducting medium, the mobile phase flows into the heat exchange coil from the liquid inlet A, exchanges heat with the heated heat-conducting medium in the process of flowing through the heat exchange coil, and the mobile phase after heat exchange flows out from the liquid outlet.
[0015] The quick-connect joint comprises a top base, a top flow plate, an upper spring, a joint male sleeve, an upper joint inner core, a nut cover, a joint female sleeve, a lower joint inner core and a bottom flow plate. The upper end of the top base is connected to the output end of the cylinder, and the lower end of the top base is sealed and connected to the upper end of the joint male sleeve. The joint male sleeve is an internal hollow structure, and the lower end inner wall of the hollow interior is an inclined surface. A top flow plate is arranged inside the joint male sleeve, and the upper joint inner core is accommodated in the joint male sleeve in a floating state. The upper sleeve of the upper joint inner core is provided with There is an upper spring, the upper end of the upper joint inner core is inserted into the central hole A of the top flow plate, and the lower end is abutted against the inclined surface of the lower end of the hollow interior of the joint male sleeve under the action of the upper spring, and a liquid flow hole is provided on the top flow plate, and a liquid inlet B connected to the liquid flow hole is provided on the top base; the joint female sleeve is connected to the liquid inlet and outlet ends of the ytterbium-converted salt column or the lutetium-converted salt column, the nut cover is sealed with the upper end of the joint female sleeve, and the lower end of the joint female sleeve is connected to the bottom flow plate screw located in the liquid inlet and outlet ends of the ytterbium-converted salt column or the lutetium-converted salt column. The bottom flow plate is an internal hollow structure, the upper inner wall of the hollow interior is an inclined surface, the lower joint inner core is in a floating state and is accommodated in the joint female sleeve, the lower joint inner core is sleeved with a lower spring, the lower end of the lower joint inner core is inserted into the center hole B of the bottom flow plate, and the upper end is in contact with the inclined surface of the upper end of the hollow interior of the joint female sleeve under the action of the lower spring; the cylinder drives the top base and the joint male sleeve to move toward the joint female sleeve until the joint male sleeve is sealed and abutted with the joint female sleeve, thereby realizing the inlet and outlet of liquid. The quick-connect joint at the end is connected, the lower end of the upper joint inner core is abutted against the upper end of the lower joint inner core, and the liquid flows to the bottom flow plate through the liquid inlet B, the liquid flow hole, the inside of the joint male sleeve, the inside of the nut cover, and the inside of the joint female sleeve of the quick-connect joint at the liquid inlet end in turn, and finally flows into the ytterbium salt column or the lutetium salt column through the gap between the lower end of the lower joint inner core and the center hole B, and after the salt conversion, it flows out through the bottom flow plate, the inside of the joint female sleeve, the inside of the nut cover, the inside of the joint male sleeve, the liquid flow hole, and the liquid inlet B of the quick-connect joint at the liquid outlet end.
[0016] The advantages and positive effects of the present invention are: 1. The present invention controls the injection system and valve components through a control terminal, and then controls the flow of liquid in the separation and purification device, so that the separation and purification column in the device separates the ytterbium-lutetium mixture to obtain fractions containing ytterbium ions and lutetium ions, and flows into the corresponding fraction tanks in the fractionation component respectively, and then the ytterbium ions and lutetium ions are post-processed by the corresponding salt conversion component to obtain corresponding ytterbium salts and lutetium salts, thereby completing the separation and purification requirements of lutetium in the ytterbium-lutetium mixture. Among them, by reasonably arranging the salt conversion component, valve component, separation and purification column, injection system, fractionation component and waste liquid component on and near the mounting frame, the various devices for separating and purifying the ytterbium-lutetium mixture are concentrated and reasonably distributed, so that the device can realize the function of separating and purifying lutetium in the ytterbium-lutetium mixture, and the volume of the overall device is small enough through reasonable and compact space arrangement and distribution.
[0017] 2. Each valve assembly of the present invention is a pneumatic valve, and the flow of each liquid in the device is achieved by pneumatics, and the electronic parts of each component are arranged outside the box, so that the components inside the box avoid the influence of radioactive decay on the life of the parts, and ensure the stability and reliability of the device as a whole. In addition, the radiation resistance of the parts is improved by adjusting the material of the parts, and the service life of the parts is guaranteed. Therefore, the present invention uses pneumatic full-automatic control, so that the entire process steps do not need to be controlled by operators, avoiding the influence of radiation on operators, and by adjusting the materials, adopting pneumatic control structure and setting the electronic parts of each component on the outside of the box for radiation resistance adjustment, the radiation resistance and service life of each component in the separation and purification device are greatly improved, and the volume of the separation and purification device is reduced through the reasonable distribution and connection of each component.
[0018] 3. The present invention provides quick-connect joints at the liquid inlet and outlet ends of the ytterbium-converted salt column and the lutetium-converted salt column, which can be connected or disconnected by a cylinder drive, making it convenient for a manipulator to replace the ytterbium-converted salt column and the lutetium-converted salt column. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention; Figure 2 It is a structural front view of the present invention; Figure 3 It is a rear view of the structure of the present invention; Figure 4 It is a left view of the structure of the present invention; Figure 5 for Figure 4 A top view of Figure 6 It is a structural principle diagram of the present invention; Figure 7 for Figure 1 Schematic diagram of the external structure of the quick-connect connector in disconnected state; Figure 8 for Figure 7 A cross-sectional view of the internal structure; Fig. 9 for Figure 1 Schematic diagram of the external structure of the medium quick-connect connector in the connected state; Fig.10 for Fig. 9 A cross-sectional view of the internal structure; Fig.11 for Figure 6 Schematic diagram of the three-dimensional structure of the heat exchanger; Fig.12 for Fig.11 The main view of the structure; Fig.13 for Fig.12 Left view without the shell; Fig.14 for Fig.12 A-A sectional view; Fig.15 for Fig.12 A top view of Among them: 1 is reagent tank A, 2 is reagent tank B, 3 is reagent tank C, 4 is reagent tank D, 5 is pump A, 6 is pump B, 7 is pump C, 8 is pump D, 9 is heat exchanger, 901 is shell, 902 is liquid inlet A, 903 is liquid outlet, 904 is heating rod, 905 is temperature sensor A, 906 is coil rack, 907 is heat exchange coil, 10 is mounting rack, 11 is frame, 12 is mounting plate A, 13 is mounting plate B, 14 is material replacement tray, 15 is cylinder, 16 is Quick-connect connector, 1601 is the top base, 1602 is the liquid inlet, 1603 is the top flow plate, 1604 is the center hole A, 1605 is the liquid hole, 1606 is the upper spring, 1607 is the sealing ring, 1608 is the joint sleeve, 1609 is the upper joint core, 1610 is the nut cover, 1611 is the joint sleeve, 1612 is the lower joint core, 1613 is the bottom flow plate, 1614 is the center hole B, 1615 is the lower spring, 20 is the salt transfer assembly, 21 is the ytterbium transfer assembly salt column, 22 is a lutetium-transfer salt column, 30 is a valve assembly, 31 is a one-way multi-way valve, 311 is a one-way four-way valve, 312 is a one-way six-way valve A, 313 is a one-way 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, 323 is a three-way valve D, 324 is a three-way valve E, 325 is a three-way valve F, 326 is a three-way valve G, 327 is a three-way valve H, 328 is a three-way valve I, 329 is a three-way valve J, 40 is a separation and purification column, 50 is a sampling system, 51 is a sampling injection pump, 52 is a six-way sampling valve, 53 is a quantitative loop, 54 is a sample tank, 60 is a fraction assembly, 61 is a lutetium fraction tank, 62 is an ytterbium fraction tank, 63 is an ytterbium finished product tank, 64 is a lutetium finished product tank, 70 is a waste liquid assembly, 71 is a first waste liquid tank, 72 is a second waste liquid tank, 73 is a third waste liquid tank, 80 is an energy spectrum detection probe, 801 is an energy spectrum detection probe A, 802 is an energy spectrum detection probe B, 90 is an ultraviolet detector, and 100 is a reaction tube. DETAILED DESCRIPTION
[0020] In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. Several embodiments of the present invention are given in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.
[0021] It should be noted that when an element is referred to as being "fixed to" another element, it may be directly on the other element or there may be a central element. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. The terms "vertical", "horizontal", "left", "right" and similar expressions used herein are for illustrative purposes only.
[0022] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which the present invention belongs. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.
[0023] like Figures 1 to 6 As shown, the present invention comprises a mounting frame 10, a salt conversion assembly 20, a valve assembly 30, a separation and purification column 40, a sampling system 50, a fractionation assembly 60, a waste liquid assembly 70, a sample tank 54, and a finished product tank, wherein the salt conversion assembly 20 comprises an ytterbium salt conversion column 21 and a lutetium salt conversion column 22, the ytterbium salt conversion column 21, the lutetium salt conversion column 22 and the separation and purification column 40 are respectively mounted on the front side of the mounting frame 10, and the separation and purification column 40 is located on one side of the salt conversion assembly 20; the liquid inlet and outlet ends of the ytterbium salt conversion column 21 and the lutetium salt conversion column 22 are both provided with quick-connect connectors 16, and the ytterbium salt conversion column 21 and the lutetium salt conversion column 22 are provided with quick-connect connectors 16. The mounting frame 10 above the lutetium-converted salt column 21 and the lutetium-converted salt column 22 is fixed with cylinders 15 of the same number and one-to-one correspondence as the quick-connect joints 16 at the liquid inlet end, and the mounting frame 10 below the ytterbium-converted salt column 21 and the lutetium-converted salt column 22 is fixed with cylinders 15 of the same number and one-to-one correspondence as the quick-connect joints 16 at the liquid outlet end, and the cylinders 15 control the switches of the corresponding quick-connect joints 16, thereby realizing the connection or disconnection between the ytterbium-converted salt column 21 and the lutetium-converted salt column 22 and the pipeline; the valve assembly 30 and the injection system 50 are respectively installed on the rear side of the mounting frame 10; the fractionation assembly 60 includes a lutetium fractionation assembly 60, a lutetium fractionation assembly 61, and a lutetium fractionation assembly 62. The lutetium fraction tank 61 and the ytterbium fraction tank 62, the lutetium fraction tank 61 is mounted on the mounting frame 10 or is arranged on one side of the mounting frame 10, and the ytterbium fraction tank 62 is arranged on one side of the mounting frame 10 or is mounted on the mounting frame 10; the waste liquid component 70 includes at least one waste liquid tank, and the waste liquid tank is mounted on the mounting frame 10 or is arranged on one side of the mounting frame 10; the front side of the mounting frame 10 is provided with an energy spectrum detection probe 80, the mounting frame 10 below the valve assembly 30 is provided with an ultraviolet detector 90, and the pipeline between the separation and purification column 40 and the waste liquid tank is respectively provided with an ultraviolet detector 90 and reaction tube 100; the sample tank 54 contains a target solution to be separated, the control terminal controls the on-off of the valve in the sampling system 50 and the valve assembly 30, controls the target solution to be separated to flow to the separation and purification column 40 for separation of ytterbium ions and lutetium ions, and 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 conversion salt column 22 for lutetium conversion salt concentration, and the ytterbium fraction in the ytterbium fraction tank 62 is introduced into the ytterbium conversion salt column 21 for ytterbium conversion salt recovery.
[0024] It can be understood that the control terminal is used to control the injection system 50 and the valve assembly 30, etc. to control the flow of liquid in the separation and purification device, so that the separation and purification column 40 separates the ytterbium-lutetium mixture to obtain an ytterbium fraction containing ytterbium ions and a lutetium fraction containing lutetium ions, and they flow into corresponding fraction tanks in the fraction assembly 60 respectively, and then the ytterbium ions and lutetium ions are post-treated by the corresponding salt conversion assembly 20 to obtain the required ytterbium salt and lutetium salt, thereby completing the separation and purification requirements of lutetium in the ytterbium-lutetium mixture and the recovery of raw ytterbium. Among them, by reasonably arranging the salt conversion component 20, the valve component 30, the separation and purification column 40, the injection system 50, the fraction component 60 and the waste liquid component 70 on the mounting frame 10 and near the mounting frame 10, the various devices for separating and purifying the ytterbium-lutetium mixture are concentrated and reasonably distributed, so that the device can realize the function of lutetium separation and purification of the ytterbium-lutetium mixture, and the overall device volume is small enough through reasonable and compact space arrangement and distribution. And in the specific implementation, the valves in each valve component 30 are all pneumatic valves, the flow of each liquid in the device is achieved by pneumatic, and the electronic parts of each component are arranged on the outside of the box, so that the components avoid the influence of radioactive decay on the life of the parts, and ensure the stability and reliability of the overall device. Therefore, the present invention uses pneumatic full-automatic control, so that the entire process step does not need to be controlled by the operator, avoiding the influence of radiation on the operator, and by adjusting the material and adopting the pneumatic control structure, the radiation resistance and service life of each component in the separation and purification device are greatly improved, and the volume of the separation and purification device is reduced through the reasonable distribution and connection of each component. Specifically: The mounting frame 10 of 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 mounted on one side of the frame 11, and a mounting plate A12 and a mounting plate B13 are mounted on the other side of the frame 11. The salt transfer component 20 is mounted on the outward side of the mounting plate A12, and the valve component 30 and the injection system 50 are mounted on the outward side of the mounting plate B13. In the specific implementation, the space in the frame 11 is reasonably divided and used to set the separation and purification column 40 and the mounting plate A12 and the mounting plate B13 respectively. Then, by reasonably adjusting the space on the mounting plate A12 and the mounting plate B13, they are used to set the salt transfer component 20, the injection system 50 and the valve component 30 respectively, so that the irregular components are arranged on the regular frame 11 through reasonable distribution, and the space is reasonably and effectively used, which greatly reduces the floor space of the overall device. In addition, a sample tank 54 and a finished product tank are arranged between the mounting plate A12 and the mounting plate B13, and the sampling system 50 is connected to the sample tank 54, the six-way sampling valve 52, the sampling injection pump 51 and the feeding device through pipelines; that is, the six-way sampling valve 52 with the quantitative loop 53 is connected to the reagent tank D4, the sample tank 54, the separation and purification column 40, and the third waste liquid tank 73 through pipelines, respectively, and the sampling injection pump 51 is arranged on the pipeline connected to the third waste liquid tank 73, and the heat exchanger 9 is arranged on the pipeline connected to the reagent tank D4. In addition, in the specific implementation, the finished product tank includes an ytterbium finished product tank 63 and a lutetium finished product tank 64, and the carrier-free lutetium-177 obtained by lutetium salt conversion concentration is discharged into the lutetium finished product tank 64, and the solution recovered by ytterbium salt conversion is discharged into the ytterbium finished product tank 63. By arranging the sample tank 54 and the finished product tank between the mounting plate A12 and the mounting plate B13, the space in the mounting frame 10 can be used as much as possible.
[0025] In this embodiment, a material replacement tray 14 is provided at the bottom of the mounting frame 10, and the material replacement tray 14 is used to hold replacement parts. Specifically, a salt transfer column, a separation and purification column 40, a valve, etc. can be placed on the material replacement tray 14. These parts are replaced, disassembled, and repaired by a manipulator. By way of example and not limitation, in some optional embodiments, the material replacement tray 14 is in the form of a seesaw. The replacement part is placed at one end, and then the manipulator presses on the other end, and the part moves close to the manipulator, and then the manipulator picks it up for replacement.
[0026] The valve components 30 of this embodiment are all pneumatic valves, including a plurality of evenly distributed three-way valves 32 and a plurality of one-position multi-way valves 31 arranged on one side of all three-way valves 32. In specific implementation, the relative positions of the three-way valve 32 and the one-position multi-way valve 31 can be adjusted according to the specific installation conditions to ensure the reasonable application of space. By setting a plurality of different valves, the flow of liquid in the device is controlled to ensure the stable and accurate operation of the production process. Specifically, a spectrum detection probe 80 is provided on the side of the mounting frame 10 close to the salt conversion component 20, and a UV detector 90 is provided below the valve component 30. The spectrum detection probe 80 and the UV detector 90 are used to monitor the outflow time of each product in the device to assist the operation of the valve component 30 and the injection system 50. In addition, a temperature sensor B is also provided on the separation and purification column 40, and the temperature sensor B is used to detect the temperature of the separation and purification column 40 to ensure that the separation and purification column 40 operates in an optimized temperature range. In addition, the installation positions of the spectrum detection probe 80 and the UV detector 90 can also be adjusted according to actual conditions to rationally utilize space, and are not limited. The three-way valves of 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 conversion salt column 21, a three-way valve D323 located at the output end of the ytterbium conversion salt column 21, a three-way valve E324 located at the input end of the lutetium conversion salt column, a three-way valve F325 located at the output end of the lutetium conversion salt column, a three-way valve G326 located on the pipeline between the three-way valve D323 and the ytterbium finished product tank 63, and a three-way valve G327 located on the pipeline between the three-way valve D327 and the ytterbium finished product tank 63. A three-way valve H327 on the pipeline between the three-way valve 325F and the lutetium finished product tank 64, a three-way valve I328 connected to the reagent tank A1 through a pipeline, and a three-way valve J329 connected to the reagent tank B2 through a pipeline. The one-position multi-way valve in this embodiment includes a four-way valve 311 located on the pipeline between the three-way valve B321 and the ytterbium fraction tank 62, a six-way valve A312 located at the input end of each lutetium fraction tank 61, and a six-way valve B313 located at the output end of each lutetium fraction tank 61.
[0027] In this embodiment, two separation and purification columns 40 are arranged side by side, and the input ends of the two separation and purification columns 40 are provided with three-way valves A320. The first interface of the three-way valve A320 is connected to the six-way injection valve 52 through a pipeline, and the second interface and the third interface 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 provided with a three-way valve B321, and the first interface of the three-way valve B321 is divided into two branches, one branch passes through the reactor 100 and the ultraviolet detector 90 to the third waste liquid tank 73, and the other branch passes through the energy spectrum detection probe A801 and the first four-way valve 311 to the ytterbium fraction tank 62, the second interface and the third interface of the three-way valve B321 are respectively connected to the output ends of the two separation and purification columns 40, and the other two interfaces of the first four-way valve 311 are respectively connected to the third waste liquid tank 73 and the input end of the first six-way valve A312 through pipelines. The filler in the separation and purification column 40 of this embodiment can be the filler prepared in Example 1 of CN102614845A published on August 1, 2012.
[0028] In this embodiment, five lutetium fraction tanks 61 and one ytterbium fraction tank 62 are provided. The five lutetium fraction tanks 61 are all provided on the top of the mounting frame 10, and one ytterbium fraction tank 62 is provided on one side of the mounting frame 10. In specific implementation, the amount of the ytterbium-lutetium mixture separated and purified each time is determined by introducing the ytterbium-lutetium mixture in the sample tank 54 into the quantitative ring 53. By providing five lutetium fraction tanks 61, when the ytterbium-lutetium mixture in one sample tank 54 enters the quantitative ring 53 in sequence for multiple separation and purification, the lutetium ions separated each time can be stored separately to ensure the independence of each separation and purification, thereby preventing errors and avoiding mutual influence of separations in different rounds. The input ends of the five lutetium fraction tanks 61 and the first waste liquid tank 71 are provided with a six-way valve A312, and the input ends of the six-way valve A312 are connected to the reagent tank A1 and the four-way valve 311 through pipelines respectively. The output ends of the five lutetium fraction tanks 61 and the first waste liquid tank 71 are provided with a six-way valve B313, and the output end of the six-way valve B313 is connected to the lutetium salt conversion column 22 through a pipeline.
[0029] The waste liquid assembly 70 of this embodiment includes a first waste liquid tank 71, a second waste liquid tank 72 and a third waste liquid tank 73. The first waste liquid tank 71 is arranged on the top of the mounting frame 10 near the side of the ytterbium fraction tank 62, the second waste liquid tank 72 and the third waste liquid tank 73 are respectively arranged on the side of the mounting frame 10, and the ytterbium fraction tank 62 is arranged on the top of the second waste liquid tank 72. The third waste liquid tank 73 is used to collect waste water when the separation and the whole device is cleaned before and after the separation. Therefore, the amount of waste water is large, and the third waste liquid tank 73 is also large, so it is set separately. The second waste liquid tank 72 and the first waste liquid tank 71 are used for collecting waste liquid in the lutetium and ytterbium salt conversion processes. The second waste liquid tank 72 can be used for collecting waste liquid in the ytterbium salt conversion process, and the first waste liquid tank 71 can be used for collecting waste liquid in the lutetium salt conversion process. The second waste liquid tank 72 and the first waste liquid tank 71 can also be used for collecting waste liquid in the ytterbium salt conversion process or both for collecting waste liquid in the lutetium salt conversion process. Because the amount of waste liquid in the lutetium and ytterbium salt conversion processes is small, and thus the volumes of the second waste liquid tank 72 and the first waste liquid tank 71 are small, the second waste liquid tank 72 is arranged at the bottom of the ytterbium fraction tank 62, and the first waste liquid tank 71 is arranged at the top of the mounting frame 10 on one side close to the ytterbium fraction tank 62. Then, according to the volume, the position distribution of each waste liquid tank is reasonably set to reduce the floor space of the overall device. In addition, in the specific implementation, by adjusting the connection of the pipeline and the control of the valve, the first waste liquid tank 71, the second waste liquid tank 72 and the third waste liquid tank 73 can be replaced with each other, and are not limited to what kind of waste liquid is collected.
[0030] In this embodiment, two ytterbium salt conversion columns 21 are arranged side by side, and two lutetium salt conversion columns 22 are arranged side by side. Two salt conversion columns are installed for ytterbium and lutetium salt conversions, respectively, to ensure that when one side of the salt conversion column is damaged or needs to be cleaned, there is a spare salt conversion column that can be put into use to ensure the stable operation of the production process. In this embodiment, the ytterbium salt conversion column 21 (PEEK chromatographic column with an inner diameter of 20 mm and a length of 150 mm) is filled with a strong cation exchange resin (DOWEX® 50WX8 cation exchange resin), and the lutetium salt conversion column 22 (PEEK chromatographic column with an inner diameter of 4.6 mm and a length of 100 mm) is filled with a strong cation exchange resin (DOWEX® 50WX8 cation exchange resin).
[0031] In order to facilitate the replacement of the ytterbium salt column 21 and the lutetium salt column 22 by the manipulator instead of manual operation and reduce the requirements for the manipulator, in this embodiment, four quick connectors 16 are respectively provided at the liquid inlet end of the two ytterbium salt columns 21 and the two lutetium salt columns 22, and four quick connectors 16 are also respectively provided at the liquid outlet end of the two ytterbium salt columns 21 and the two lutetium salt columns 22, and four cylinders 15 are installed on the frame 11 above the two ytterbium salt columns 21 and the two lutetium salt columns 22, and four cylinders 15 are installed on the frame 11 below the two ytterbium salt columns 21 and the two lutetium salt columns 22, and each cylinder is connected to a control terminal, and the control terminal controls each cylinder 15 to control the corresponding quick connector 16 to disconnect or connect. Figures 7-10As shown, the quick-connect connector 16 of this embodiment includes a top base 1601, a top flow plate 1603, an upper spring 1606, a sealing ring 1607, a joint male sleeve 1608, an upper joint inner core 1609, a nut cover 1610, a joint female sleeve 1611, a lower joint inner core 1612 and a bottom flow plate 1613. The upper end of the top base 1601 is connected to the output end of the cylinder 15, and the lower end of the top base 1601 is threadedly connected to the upper end of the joint male sleeve 1608 and sealed by the sealing ring 1607. The joint male sleeve 1608 is an internal hollow structure, and the inner wall of the lower end of the hollow interior is an inclined surface inclined inward from top to bottom. A top flow plate 1603 is provided at the upper end of the hollow interior of the male sleeve 1608, a center hole A1604 is provided in the middle of the top flow plate 1603, and a plurality of liquid holes 1605 are provided in the circumferential direction around the center hole A1604; a liquid inlet B1602 for connecting to a pipeline is provided radially on the top base 1601, the liquid inlet B1602 of the quick-connect joint 16 at the liquid inlet end of the ytterbium-converted salt column 21 is connected to the three-way valve C322 through a pipeline, the liquid inlet B1602 of the quick-connect joint 16 at the liquid outlet end of the ytterbium-converted salt column 21 is connected to the three-way valve D323 through a pipeline, and the liquid inlet B1602 of the quick-connect joint 16 at the liquid inlet end of the lutetium-converted salt column 22 is connected to the three-way valve D323 through a pipeline. The liquid inlet B1602 of the quick-connect joint 16 at the liquid outlet of the lutetium transfer salt column 22 is connected to the three-way valve F325 through a pipeline; the liquid inlet B1602 is connected to the upper end of each liquid flow hole 1605 through the channel inside the top base 1601, and the lower end of each liquid flow hole 1605 is connected to the inside of the joint male sleeve 1608; the center hole A1604 on the top flow plate 1603 axially penetrates the top flow plate 1603, and the center hole A1604 is a stepped hole; the upper joint inner core 1609 is accommodated in the joint male sleeve 1608 in a floating state, and an upper spring 160 is sleeved on the upper joint inner core 1609 6. The upper end of the upper spring 1606 abuts against the lower surface of the top flow plate 1603, and the lower end of the upper spring 1606 abuts against the boss on the upper joint core 1609. The upper end of the upper joint core 1609 is inserted into the center hole A1604 of the top flow plate 1603. Under the action of the upper spring 1606, the lower end of the upper joint core 1609 abuts against the inclined surface of the lower end of the hollow interior of the joint male sleeve 1608. A sealing ring 1607 is also provided at the lower end of the upper joint core 1609. When the quick connector 16 is in a disconnected state, the upper joint core 1609 is sealed by the sealing ring 1607 and the inclined surface of the lower end of the hollow interior of the joint male sleeve 1608.
[0032] The female joint sleeve 1611 is connected to the liquid inlet and outlet ends of the ytterbium-converted salt column 21 or the lutetium-converted salt column 22, the nut cover 1610 is threadedly connected to the upper end of the female joint sleeve 1611, and is sealed by the sealing ring 1607, and the lower end of the female joint sleeve 1611 is threadedly connected to the bottom flow plate 1613 located in the liquid inlet and outlet ends of the ytterbium-converted salt column 21 or the lutetium-converted salt column 22; the bottom flow plate 1613 is an internal hollow structure, and a center hole B1614 is opened at the bottom, and the upper end inner wall of the hollow interior is an inclined surface inclined inward from bottom to top, and the lower joint core 1612 is accommodated in the female joint sleeve 1611 in a floating state, and the lower joint core 16 A lower spring 1615 is sleeved on 12, the lower end of the lower spring 1615 abuts against the bottom surface of the hollow interior of the bottom flow plate 1613, the upper end of the lower spring 1615 abuts against the boss on the lower joint inner core 1612, the lower end of the lower joint inner core 1612 is inserted into the center hole B1614 of the bottom flow plate 1613, and the upper end of the lower joint inner core 1612 abuts against the inclined surface of the upper end of the hollow interior of the joint female sleeve 1611 under the action of the lower spring 1615; when the quick connector 16 is in the disconnected state, the lower joint inner core 1612 is sealed with the inclined surface of the upper end of the hollow interior of the joint female sleeve 1611 through the sealing ring 1607.
[0033] The control terminal controls the cylinder 15 to work, and the cylinder 15 drives the top base 1601 and the joint male sleeve 1608 to move toward the joint female sleeve 1611, until the joint male sleeve 1608 and the joint female sleeve 1611 are sealed and abutted, thereby realizing the connection of the quick-connect joint 16 at the inlet and outlet ends, and the lower end of the upper joint inner core 1609 abuts against the upper end of the lower joint inner core 1612, and the channel is connected under the action of the upper spring 1606 and the lower spring 1615, and the liquid entering from the liquid inlet port B1602 of the quick-connect joint 16 at the liquid inlet end is sequentially discharged through the liquid outlet. The liquid flows through the hole 1605, the inside of the joint male sleeve 1608, the inside of the nut cover 1610, and the inside of the joint female sleeve 1611 to the inside of the bottom flow plate 1613, and finally flows into the ytterbium salt column 21 or the lutetium salt column 22 through the gap between the lower end of the lower joint inner core 1612 and the center hole B1614. After the salt conversion, it flows out through the inside of the bottom flow plate 1613 of the quick-connect joint 16 at the liquid outlet end, the inside of the joint female sleeve 1611, the inside of the nut cover 1610, the inside of the joint male sleeve 1608, the liquid hole 1605, and the liquid inlet B1602.
[0034] In this embodiment, reagent tank A1, reagent tank B2, reagent tank C3 and reagent tank D4 are respectively provided, and pumps A5, pump B6, pump C7 and pump D8 are respectively provided on the outlet pipelines of reagent tank A1, reagent tank B2, reagent tank C3 and reagent tank D4.
[0035] By way of example and not limitation, in some optional embodiments, the specific use process of the present invention is as follows: First, the mobile phase (such as eluent or eluent) in the reagent tank D4 is controlled by the injection system 50 to flush the entire device at a preset flow rate. The flow path is as follows: the feeding device delivers the mobile phase, which is heated by the heat exchanger 9 and then enters any separation and purification column 40 through the injection system 50, the six-way injection valve 52, and the three-way valve A320. After flowing out through the three-way valve B321, it is divided into two branches. A small amount of the branch (less than 3% of the total flow rate) passes through the reaction tube 100 and reacts with the color developer and flows into the ultraviolet detector 90. After detection, it is discharged into the third waste liquid tank 73 and treated as waste liquid; the main branch (greater than 97% of the total flow rate) is detected by the energy spectrum detection probe A801 and then discharged into the third waste liquid tank 73 through the first four-way valve 311. The reagent tank C3 of this embodiment contains a color developer, and the color developer in the reagent tank C3 is continuously transported to the reaction tube 100 by the pump C7.
[0036] like Figures 11 to 15 As shown, the heat exchanger 9 of this embodiment includes a shell 901, a heating rod 904, a temperature sensor A905, a coil rack 906 and a heat exchange coil 907. The shell 901 is filled with a heat-conducting medium (the heat-conducting medium of this embodiment can be water or heat-conducting oil). The top of the shell 901 is respectively provided with a liquid inlet A902 and a liquid outlet 903. The shell 901 is internally installed with a coil rack 906. The heat exchange coil 907 is spirally wound on the coil rack 906. The two ends of the heat exchange coil 907 are respectively connected with the liquid inlet A902 and the liquid outlet 903; A heating rod 904 and a temperature sensor A905 are respectively provided inside the tube rack 906. The heating rod 904, the temperature sensor A905, the coil rack 906 and the heat exchange coil 907 are all immersed in a heat-conducting medium. The upper ends of the heating rod 904 and the temperature sensor A905 are fixed on the outer shell 901. The heating rod 904 is energized to heat the heat-conducting medium. The mobile phase flows into the heat exchange coil 907 from the liquid inlet A902, exchanges heat with the heated heat-conducting medium in the process of flowing through the heat exchange coil 907, and the mobile phase after heat exchange flows out from the liquid outlet 903.
[0037] The control terminal controls the six-way injection valve 52 to switch, so that the ytterbium-lutetium mixture in the sample tank 54 is pumped into the quantitative ring 53, and then the six-way injection valve 52 is switched again, and the mobile phase in the reagent tank D4 is pumped in by the injection pump 51, and the sample can be brought into the separation and purification column 40 by the mobile phase, and the separation process officially begins. The final destination of the main flow depends on the signals of the energy spectrum detection probe A801 and the ultraviolet detector 90. According to the signals provided by the energy spectrum detection probe A801 and the ultraviolet detector 90, the switching of the first four-way valve 311 is controlled. When the signal of lutetium is detected, it flows to the lutetium fraction tank 61 through the first six-way valve A312 (limited by the hot chamber space, this embodiment can be separated up to five times. To prevent errors, the lutetium fraction is collected separately each time, so five lutetium fraction tanks 61 are equipped. The number of lutetium fraction tanks does not affect the development of this separation process); when the ytterbium signal is detected, it flows to the ytterbium fraction tank 62; in other cases, it flows to the third waste liquid tank 73. After the separation is completed, the separation and purification column 40 can be cleaned and preserved with 10% to 100% methanol; it is also possible not to preserve it, which can be determined according to the characteristics of the separation and purification column 40.
[0038] The separated lutetium fraction contains organic acid eluent, which does not meet the requirements of final use. Therefore, it is necessary to carry out a salt conversion and concentration step for lutetium. This step can not only remove the eluent and convert it into a lutetium chloride solution that meets medical use, but also achieve the effect of concentrating the lutetium product (the separated lutetium fraction is very dilute). Specifically: Device replacement: The water in the reagent tank B2 is used to replace the storage solution in the device through the feeding equipment, and the water flows through the three-way valve J329, the three-way valve E324, the lutetium conversion salt column 22, the three-way valve F325, the energy spectrum detection probe B802, the three-way valve H327, and the first six-way valve A312 and then discharged into the first waste liquid tank 71; Sample preparation: The 2M hydrochloric acid in the reagent tank A1 is sequentially injected into the lutetium fraction tank 61 containing the lutetium fraction through the first six-way valve A312, and then the liquid is evenly mixed by gas stirring; Loading: The liquid in the above lutetium fraction tank 61 is sequentially loaded into the lutetium conversion salt column 22 through the first six-way valve B313 and the three-way valve E324, and the lutetium ions are adsorbed in the lutetium conversion salt column 22. If the sample is loaded by pump, the radiation will damage the circuit board of the pump and cause the device to fail. Considering the radiation protection, the sample is loaded by gas pressure in this device, and the liquid can also be transferred by pump; elution: the water in the reagent tank B2 is sent to the lutetium salt column 22 through the three-way valve J329 and the three-way valve E324 to remove the organic acid eluent remaining in the lutetium salt column 22, and the waste liquid is discharged into the first waste liquid tank 71 through the three-way valve F325, the three-way valve H327 and the first six-way valve A312; elution: the reagent tank A 1 is manually replaced with 0.15 mM hydrochloric acid, and 0.15 mM hydrochloric acid is pumped into the lutetium salt conversion column 22 through pump A5, three-way valve I328, and three-way valve E324, and the lutetium ions adsorbed in the lutetium salt conversion column 22 are washed with 0.15 mM hydrochloric acid to obtain a concentrated lutetium chloride solution, which is then collected into the lutetium finished product tank 64 after passing through three-way valve F325 and three-way valve H327; after the lutetium salt conversion is concentrated, the product can be transferred to the desired place; the lutetium salt conversion column 22 can be regenerated and stored as needed.
[0039] The separated ytterbium fraction contains organic acid eluent, which is not conducive to precipitation and recovery, so the ytterbium needs to be subjected to a salt conversion and concentration step. This step can remove the eluent and convert it into ytterbium chloride solution, which is convenient for subsequent further precipitation and calcination into ytterbium oxide (recycled as a target material raw material). Specifically: Device replacement: The water in the reagent tank B2 is used to replace the storage solution in the device through the feeding device, and the water flows through the three-way valve J329, the three-way valve C322, the ytterbium salt column 21, the three-way valve D323, and the three-way valve G326 and then discharged into the second waste liquid tank 72; Sample preparation: 2M hydrochloric acid in the reagent tank A1 is pumped into the ytterbium fraction tank 62 containing the ytterbium fraction through the pump A5, and then the liquid is evenly mixed by gas stirring; Sample loading: The liquid in the above ytterbium fraction tank 62 is loaded into the ytterbium salt column 21 through the three-way valve J329 and the three-way valve C322, so that the ytterbium ions are adsorbed in the ytterbium salt column 21; Rinse: Use the reagent tank B2 Water passes through three-way valve J329 and three-way valve C322 to the ytterbium salt conversion column 21 to remove the organic acid eluent remaining in the ytterbium salt conversion column 21, and the waste liquid is discharged into the second waste liquid tank 72 through three-way valve D323 and three-way valve G326; Elution: manually replace the reagent tank A1 with 0.15mM hydrochloric acid, and pump 0.15mM hydrochloric acid into the ytterbium salt conversion column 21 through pump A5 through three-way valve I328 and three-way valve C322, and use 0.15mM hydrochloric acid to wash off the ytterbium ions adsorbed in the ytterbium salt conversion column 21, and obtain a high-purity ytterbium chloride solution, which is then collected in the ytterbium finished product tank 63 after passing through three-way valve D323 and three-way valve G326. After the ytterbium salt recovery is completed, the product is transferred to the desired location, and then the precipitation and calcination processes are continued to obtain ytterbium oxide powder. According to the needs, the ytterbium salt column 21 is regenerated and preserved.
[0040] In addition, 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, which is used to run the program code stored in the memory or process data, such as executing an access restriction program. In some embodiments, the memory includes at least one type of readable storage medium, and the readable storage medium includes a flash memory, a hard disk, a multimedia card, a card-type memory (for example, SD or DX memory, etc.), a magnetic memory, a disk, an optical disk, etc. In some embodiments, the memory may be an internal storage unit of an electronic device, such as a hard disk of the electronic device. In other embodiments, the memory may also be an external storage device of an electronic device, such as a plug-in hard disk equipped on the electronic device, a smart memory card (SmartMedia Card, SMC), a secure digital (Secure Digital, SD) card, a flash card (Flash Card), etc. Further, the memory may also include both an internal storage unit and an external storage device 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 is to be output.
[0041] In addition, the device of the present invention also includes a seal, which is used to seal the parts in the device of the present invention, and the material of the seal is a radiation-resistant material. By way of example and not limitation, in some optional embodiments, a seal is usually provided on the connection or pneumatic valve of the device of the present invention, and then by using a radiation-resistant material for the seal, the life of the part can be effectively extended. It should be noted that, through the use process of the above-mentioned device, it can be seen that the present invention realizes the fully automatic separation and purification function of the ytterbium-lutetium mixture by reasonably automatically controlling the on-off of the valve and the flow of the liquid, so that the device can be fully automated to avoid irradiation of the staff, and improves the production efficiency. In addition, the device of the present invention adopts an integrated design, so that the automated operation can be realized in a smaller space, reducing the cost of large-scale automated control, so that the automated control of the present invention can meet the actual production cost situation. In addition, in order to avoid the influence of irradiation on the life of the device, the design and processing of the present invention fully consider the radiation resistance, such as the sealing ring is replaced from ordinary polytetrafluoroethylene rubber to ethylene propylene rubber, the electronic control mechanism in the device is replaced by a pneumatic control mechanism, and the liquid transfer inside the hot chamber is controlled by air pressure.
[0042] In summary, a separation and purification device in the above-mentioned embodiment of the present invention controls the injection system 50 and the valve assembly 30 through the control terminal to control the flow of the liquid in the separation and purification device, so that the separation and purification column 40 separates the ytterbium-lutetium mixture to obtain fractions containing ytterbium ions and lutetium ions and flow them into the corresponding fraction tanks in the fraction assembly 60 respectively, and then the ytterbium ions and lutetium ions are post-processed through the corresponding salt conversion assembly 20 to obtain the required ytterbium salt and lutetium salt, thereby completing the separation and purification requirements of lutetium in the ytterbium-lutetium mixture and the recovery requirements of the raw material ytterbium. Among them, by reasonably arranging the salt conversion component 20, the valve component 30, the separation and purification column 40, the injection system 50, the fractionation component 60 and the waste liquid component 70 on the mounting frame 10 and near the mounting frame 10, the various devices for separating and purifying the ytterbium-lutetium mixture are concentrated and reasonably distributed, so that the device can realize the function of lutetium separation and purification of the ytterbium-lutetium mixture, and the volume of the overall device is small enough through reasonable and compact space arrangement and distribution. And in the specific implementation, the valves in each valve component 30 are pneumatic valves, and the flow of each liquid in the device is achieved pneumatically. Therefore, the present invention uses pneumatic full-automatic control, so that the entire process steps do not need to be controlled by the operator, avoiding the impact of radiation on the operator, and by adjusting the materials and adopting the pneumatic control structure, the radiation resistance and service life of each component in the separation and purification device are greatly improved, and the volume of the separation and purification device is reduced through the reasonable distribution and connection of each component.
[0043] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.
[0044] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present invention. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
Claims
1. A device for separation and purification of carrier-free lutetium-177, characterized in that: The invention comprises a mounting frame (10), a salt conversion assembly (20), a valve assembly (30), a separation and purification column (40), a sample injection system (50), a fraction assembly (60), a waste liquid assembly (70), a sample tank (54) and a finished product tank, wherein the salt conversion assembly (20) comprises an ytterbium salt conversion column (21) and a lutetium salt conversion column (22), the ytterbium salt conversion column (21), the lutetium salt conversion column (22) and the separation and purification column (40) are respectively mounted on the front side of the mounting frame (10), and the separation and purification column (40) is located on one side of the salt conversion assembly (20); the liquid inlet and outlet ends of the ytterbium salt conversion column (21) and the lutetium salt conversion column (22) are both provided with quick-connect joints (16); the ytterbium salt conversion column (21) and the lutetium salt conversion column (22) are ... The mounting frame (10) above the ytterbium-converted salt column (21) and the lutetium-converted salt column (22) is fixed with cylinders (15) of the same number and one-to-one correspondence as the quick-connect joints (16) at the liquid inlet end; the mounting frame (10) below the ytterbium-converted salt column (21) and the lutetium-converted salt column (22) is fixed with cylinders (15) of the same number and one-to-one correspondence as the quick-connect joints (16) at the liquid outlet end; the cylinders (15) control the switches of the corresponding quick-connect joints (16), thereby realizing the connection or disconnection between the ytterbium-converted salt column (21) and the lutetium-converted salt column (22) and the pipeline; the valve assembly (30) and the injection system (50) are respectively mounted on the rear side of the mounting frame (10); the fraction assembly (60) comprises A lutetium fraction tank (61) and an ytterbium fraction tank (62), wherein the lutetium fraction tank (61) is mounted on a mounting frame (10) or arranged on one side of the mounting frame (10), and the ytterbium fraction tank (62) is arranged on one side of the mounting frame (10) or mounted on the mounting frame (10); the waste liquid assembly (70) comprises at least one waste liquid tank, wherein the waste liquid tank is mounted on the mounting frame (10) or arranged on one side of the mounting frame (10); an energy spectrum detection probe (80) is arranged on the front side of the mounting frame (10), an ultraviolet detector (90) is arranged on the mounting frame (10) below the valve assembly (30), and a separation and purification column (40) is arranged on the pipeline between the separation and purification column (40) and the waste liquid tank. A UV detector (90) and a reaction tube (100) are separately provided; the sample tank (54) contains a target material solution to be separated; the control terminal controls the on / off of the valve in the sample injection system (50) and the valve assembly (30) to control the target material solution to be separated to flow to the separation and purification column (40) to separate ytterbium ions and lutetium ions; the lutetium fraction containing lutetium ions after separation is collected in the lutetium fraction tank (61); 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 transsalt column (22) for lutetium transsalt concentration; and the ytterbium fraction in the ytterbium fraction tank (62) is introduced into the ytterbium transsalt column (21) for ytterbium transsalt recovery.
2. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The mounting frame (10) comprises a frame (11), a mounting plate A (12), and a mounting plate B (13); the frame (11) is the main body of the mounting frame (10); a separation and purification column (40) is mounted on one side of the frame (11); and a mounting plate A (12) and a mounting plate B (13) arranged in front and behind are mounted on the other side of the frame (11); the salt conversion assembly (20) is mounted on the outward side of the mounting plate A (12); and the valve assembly (30) and the injection system (50) are mounted on the outward side of the mounting plate B (13); and the sample tank (54) and the finished product tank are respectively arranged between the mounting plate A (12) and the mounting plate B (13).
3. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: A material replacement tray (14) for containing parts is provided at the bottom of the mounting frame (10).
4. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The lutetium fraction tank (61) is one or more and is installed on the top of the mounting frame (10), and the ytterbium fraction tank (62) is arranged on one side of the mounting frame (10).
5. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The waste liquid assembly (70) comprises a first waste liquid tank (71), a second waste liquid tank (72) and a third waste liquid tank (73); the first waste liquid tank (71) is mounted on the top of a mounting frame (10); the second waste liquid tank (72) and the third waste liquid tank (73) are respectively arranged on one side of the mounting frame (10); and the ytterbium fraction tank (62) is arranged on the top of the second waste liquid tank (72).
6. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The ytterbium-converted salt column (21) is one or a plurality of columns arranged side by side, and the lutetium-converted salt column (22) is one or a plurality of columns arranged side by side.
7. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The injection system (50) comprises an injection pump (51) and a six-way injection valve (52) with a quantitative loop (53); the six-way injection valve (52) is connected to a sample tank (54), a separation and purification column (40), a waste liquid tank and a mobile phase through pipelines, respectively; and the injection pump (51) is arranged on the pipeline.
8. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The finished product tank comprises an ytterbium finished product tank (63) and a lutetium finished product tank (64). The carrier-free lutetium-177 obtained by lutetium transsalting and concentration is discharged into the lutetium finished product tank (64), and the solution recovered by ytterbium transsalting is discharged into the ytterbium finished product tank (63).
9. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The device is cleaned before separation and purification, and the mobile phase transported by the feeding device is heated by the heat exchanger (9) and then enters the device; the heat exchanger (9) comprises a shell (901), a heating rod (904), a temperature sensor A (905), a coil rack (906) and a heat exchange coil (907); a heat-conducting medium is filled in the shell (901); a liquid inlet A (902) and a liquid outlet (903) are respectively provided on the top of the shell (901); a coil rack (906) is installed inside the shell (901); a heat exchange coil (907) is wound around the coil rack (906); two ends of the heat exchange coil (907) are respectively connected to the liquid inlet A (902) and the liquid outlet (903) is connected; a heating rod (904) and a temperature sensor A (905) are respectively provided inside the coil rack (906); the heating rod (904), the temperature sensor A (905), the coil rack (906) and the heat exchange coil (907) are all immersed in a heat-conducting medium; the upper ends of the heating rod (904) and the temperature sensor A (905) are fixed on the housing (901); the heating rod (904) is energized to heat the heat-conducting medium; the mobile phase flows into the heat exchange coil (907) from the liquid inlet A (902), exchanges heat with the heated heat-conducting medium in the process of flowing through the heat exchange coil (907), and the mobile phase after heat exchange flows out from the liquid outlet (903).
10. The device for separation and purification of carrier-free lutetium-177 according to claim 1, characterized in that: The quick-connect joint (16) comprises a top base (1601), a top flow plate (1603), an upper spring (1606), a joint male sleeve (1608), an upper joint inner core (1609), a nut cover (1610), a joint female sleeve (1611), a lower joint inner core (1612) and a bottom flow plate (1613). The upper end of the top base (1601) is connected to the output end of the cylinder (15), the lower end of the top base (1601) is sealed to the upper end of the joint male sleeve (1608), and the joint male sleeve (1608) is The inner wall of the lower end of the hollow interior is an inclined surface, the interior of the joint male sleeve (1608) is provided with a top flow plate (1603), the upper joint inner core (1609) is accommodated in the joint male sleeve (1608) in a floating state, the upper joint inner core (1609) is provided with an upper spring (1606), the upper end of the upper joint inner core (1609) is inserted into the center hole A (1604) of the top flow plate (1603), and the lower end is connected to the lower end of the hollow interior of the joint male sleeve (1608) under the action of the upper spring (1606). The inclined surfaces are abutted, the top flow plate (1603) is provided with a liquid flow hole (1605), and the top base (1601) is provided with a liquid inlet B (1602) connected to the liquid flow hole (1605); the female joint sleeve (1611) is connected to the liquid inlet and outlet ends of the ytterbium salt column (21) or the lutetium salt column (22), the nut cover (1610) is sealedly connected to the upper end of the female joint sleeve (1611), and the lower end of the female joint sleeve (1611) is connected to the bottom flow plate (1603) located in the liquid inlet and outlet ends of the ytterbium salt column (21) or the lutetium salt column (22). 1613) threaded connection, the bottom flow plate (1613) is an internal hollow structure, the upper inner wall of the hollow interior is an inclined surface, the lower joint inner core (1612) is accommodated in the joint female sleeve (1611) in a floating state, the lower joint inner core (1612) is sleeved with a lower spring (1615), the lower end of the lower joint inner core (1612) is inserted into the center hole B (1614) of the bottom flow plate (1613), and the upper end abuts against the inclined surface of the upper end of the hollow interior of the joint female sleeve (1611) under the action of the lower spring (1615);The cylinder (15) drives the top base (1601) and the joint male sleeve (1608) to move toward the joint female sleeve (1611) until the joint male sleeve (1608) and the joint female sleeve (1611) are sealed and abutted, thereby realizing the connection between the quick-connect joint (16) at the liquid inlet and outlet ends, and the lower end of the upper joint inner core (1609) abuts against the upper end of the lower joint inner core (1612), and the liquid flows through the liquid inlet port B (1602) of the quick-connect joint (16) at the liquid inlet end, the liquid outlet hole (1605), the inside of the joint male sleeve (1608), and the nut cover in sequence. (1610), the inside of the female joint sleeve (1611) to the inside of the bottom flow plate (1613), and finally flows into the ytterbium salt column (21) or the lutetium salt column (22) through the gap between the lower end of the lower joint inner core (1612) and the center hole B (1614), and then flows out through the inside of the bottom flow plate (1613) of the quick-connect joint (16) at the liquid outlet end, the inside of the female joint sleeve (1611), the inside of the nut cover (1610), the inside of the male joint sleeve (1608), the liquid outlet hole (1605), and the liquid inlet B (1602). ;
Citation Information
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