CN117594277A - Enrichment from reactor irradiation 46 Extracting Ca target material 47 Sc device and method - Google Patents
Enrichment from reactor irradiation 46 Extracting Ca target material 47 Sc device and method Download PDFInfo
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- CN117594277A CN117594277A CN202311563500.1A CN202311563500A CN117594277A CN 117594277 A CN117594277 A CN 117594277A CN 202311563500 A CN202311563500 A CN 202311563500A CN 117594277 A CN117594277 A CN 117594277A
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- 239000013077 target material Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 87
- 238000000926 separation method Methods 0.000 claims abstract description 83
- 239000007924 injection Substances 0.000 claims abstract description 46
- 238000002347 injection Methods 0.000 claims abstract description 46
- 239000002699 waste material Substances 0.000 claims abstract description 24
- 238000003860 storage Methods 0.000 claims abstract description 21
- 238000002386 leaching Methods 0.000 claims abstract description 19
- 239000003480 eluent Substances 0.000 claims abstract description 8
- 238000004891 communication Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 238000000605 extraction Methods 0.000 claims description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims 2
- 125000003368 amide group Chemical group 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 4
- 238000005086 pumping Methods 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 description 29
- 230000000694 effects Effects 0.000 description 17
- 239000012535 impurity Substances 0.000 description 12
- 238000001994 activation Methods 0.000 description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 9
- 239000004696 Poly ether ether ketone Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 9
- 229920002530 polyetherether ketone Polymers 0.000 description 9
- 230000004913 activation Effects 0.000 description 8
- 238000003745 diagnosis Methods 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000012795 verification Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 229910052745 lead Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 238000012827 research and development Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000005251 gamma ray Effects 0.000 description 3
- 229910052732 germanium Inorganic materials 0.000 description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- DVMZCYSFPFUKKE-UHFFFAOYSA-K scandium chloride Chemical compound Cl[Sc](Cl)Cl DVMZCYSFPFUKKE-UHFFFAOYSA-K 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001408 amides Chemical group 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000009206 nuclear medicine Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 206010006002 Bone pain Diseases 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000004816 paper chromatography Methods 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- SIXSYDAISGFNSX-NJFSPNSNSA-N scandium-47 Chemical compound [47Sc] SIXSYDAISGFNSX-NJFSPNSNSA-N 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002603 single-photon emission computed tomography Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21G—CONVERSION OF CHEMICAL ELEMENTS; RADIOACTIVE SOURCES
- G21G1/00—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes
- G21G1/02—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes in nuclear reactors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for enriching from reactor irradiation 46 Extracting Ca target material 47 The Sc device and method relate to the technical field of radioisotope preparation, comprising a shielding box body, wherein a target material dissolving tank, a decay tank, a waste liquid tank, a sample tank, a separation column, a liquid tank to be recovered and an injection pump are arranged in the shielding box body; the decay tank, the waste liquid tank and the sample tank are communicated with the separation column; the separation column, the target material dissolving tank and the decay tank are communicated with the injection pump; the injection pump has the functions of liquid pumping and liquid discharging; the outside of the shielding box body is connected with a constant flow pump communicated with the target material dissolving tank and the separation column, and the constant flow pump is connected with a leaching/dissolving liquid storage tank and an eluent storage tank through a conveying pipeline. The external part of the shielding box body is connected with a remote controller which is in communication connection with the constant flow pump, the injection pump and the electromagnetic three-way valve; can realize the function similar to the generator and improve 47 The yield of Sc has a certain degree of automation, and can reduce personnel misoperation and irradiated dose.
Description
Technical Field
The invention relates to the technical field of radioisotope preparation, in particular to a method for enriching from a reactor by irradiation 46 Extracting Ca target material 47 Sc apparatus and method.
Background
Scandium-47% 47 Sc) is a low energy beta - An emitter with a half-life of 3.34 days which decays giving off a beta with an average energy of 162keV - Emitter and 159keV gamma ray (68%), with 99m The energy of the gamma rays emitted by Tc is close, and the method is suitable for in-vivo Single Photon Emission Computed Tomography (SPECT). In addition, in the case of the optical fiber, 47 sc may be isotopically substituted with Sc 44 Sc (PET nuclide) forms a diagnosis and treatment nuclide pair, ensures that the diagnosis and treatment nuclide pair has the same chemical behavior in a human body in the diagnosis and treatment processes, and is a diagnosis and treatment integrated radionuclide. Free form 47 Sc (PET nuclide) forms a diagnosis and treatment nuclide pair, ensures that the diagnosis and treatment nuclide pair has the same chemical behavior in a human body in the diagnosis and treatment processes, and is a diagnosis and treatment integrated radionuclide. Free form 47 Sc is ingested in the animals following injection, up to bone, tumor, liver, spleen, kidney in turn, and therefore, 47 sc is expected to become a novel bone pain treatment drug.
At present, there is no provision in China 47 Related reports of Sc preparation are that small batches of Sc are prepared by various methods abroad 47 Sc is used for research of labeled drugs, and mass production is not performed yet. The method comprises two modes of accelerator activation and reactor activation, wherein the reactor activation is divided into thermal neutron activation and fast neutron activation, and the accelerator activation has the advantages of multiple selectable target materials, multiple accelerator numbers and the like, but the auxiliary activation processHas multiple reactions and easy generation 46 Sc equivalent half-life impurity 47 Sc yield is low. Fast neutron activation 47 Ti is used as a target, and the titanium alloy is prepared, 47 the yield of Sc is affected by the fast neutron energy, which, when low, 47 sc activity is difficult to meet medical requirements, and too high fast neutron energy can lead to 46 The Sc yield is too high to make the nuclear purity unsatisfactory.
Thus, at present 47 The Sc preparation mode has the advantages of multiple side reactions in the activation process and easy generation 46 Sc equivalent half-life impurity 47 The Sc yield is low, and the medical requirements are difficult to meet.
Disclosure of Invention
The technical problem to be solved by the invention is that 47 The Sc preparation mode has the advantages of multiple side reactions in the activation process and easy generation 46 Sc equivalent half-life impurity 47 The Sc yield is low and the medical requirements are difficult to meet, and the purpose is to provide a method for enriching from the radiation of a reactor 46 Extracting Ca target material 47 Sc device and method, the device can realize the function similar to a generator and improve 47 The yield of Sc has certain degree of automation, can reduce personnel misoperation and irradiation dose, and can obtain high-quality scandium chloride through the device 47 Sc) solution for providing raw materials for nuclear medicine research and development personnel in China for 47 Sc-marked compound and biological experimental study 47 The pace of research and development of Sc marked medicines improves the innovation capability of medical isotopes in China.
The invention is realized by the following technical scheme:
in one aspect, the present application provides an apparatus for irradiation enrichment from a reactor 46 Extracting Ca target material 47 The Sc device comprises a shielding box body, wherein a target material dissolving tank, a decay tank, a waste liquid tank, a sample tank, a liquid tank to be recovered, a separation column, an injection pump and a split charging device are arranged in the shielding box body;
the decay tank, the waste liquid tank and the sample tank are communicated with the separation column;
the separation column, the target material dissolving tank, the decay tank and the liquid tank to be recovered are all communicated with the injection pump;
the injection pump has the functions of liquid pumping and liquid discharging;
the three-way valves are electromagnetic three-way valves;
the outside of the shielding box body is connected with a constant flow pump communicated with the target material dissolving tank and the separation column, and the constant flow pump is connected with a leaching/dissolving liquid storage tank and an eluent storage tank through a conveying pipeline.
The external of the shielding box body is connected with a remote controller which is in communication connection with the injection pump, the constant flow pump and the electromagnetic three-way valve;
the target material dissolving tank in the device is used for dissolving the irradiated calcium carbonate target material, and high-concentration hydrochloric acid in the leaching/dissolving liquid storage tank can be selectively introduced into the target material dissolving tank by the constant flow pump for dissolving the calcium carbonate target material; filtering the target dissolving solution in the target dissolving tank, and introducing the filtered target dissolving solution into a separation column by a syringe pump 47 Ca/ 47 Sc separation; in the leaching/dissolving liquid storage tank, high-concentration hydrochloric acid can be introduced into the separation column by a constant flow pump for leaching and removing redundant calcium besides being used for dissolving target materials; the eluent storage tank is used for storing low-concentration hydrochloric acid and is introduced into the separation column by a constant flow pump for carrying out 47 Eluting Sc; after the substances in the decay tank decay for a certain time, the substances are pumped into the separation column by the injection pump for re-extraction.
Wherein, all the pipelines involved in the device adopt polyether ether ketone (PEEK) pipes. The polyether-ether-ketone tube has excellent chemical stability, can resist all strong acid, strong alkali and strong oxidant, does not react with various organic solvents, and has good irradiation resistance stability. Therefore, the polyether-ether-ketone tube is used, so that the service life of the tube is longer, and new impurities are avoided from being generated due to the action of the extraction material and the tube in the extraction process.
Wherein, be provided with the manipulator in the shielding work box.
Further, a first three-way valve is connected to the pipeline between the top of the separation column and the constant flow pump, one interface of the first three-way valve is used for connecting the pipeline communicated with the constant flow pump, the other interface is used for connecting the pipeline communicated with the separation column, and the last interface is used for connecting the branch pipe communicated with the injection pump and the liquid tank to be recovered.
The first three-way valve is connected to the pipeline between the top of the separation column and the constant flow pump, so that the liquid flowing out of the constant flow pump can enter the separation column after passing through the first three-way valve, and meanwhile, the liquid can be injected into the separation column through the injection pump.
Further, the branch pipe is provided with two branch pipes, one branch pipe is used for being connected with a liquid tank to be recovered, the other branch pipe is used for being connected with a syringe pump, and the joint of the branch pipe and the branch pipe of the liquid tank to be recovered is connected with the syringe pump through a second three-way valve.
The second three-way valve is connected to the pipeline between the top of the separation column and the liquid tank to be recovered, so that the liquid flowing out of the injection pump can enter the separation column after passing through the second three-way valve, and meanwhile, the liquid can be injected into the liquid tank to be recovered through the injection pump.
Further, a third three-way valve is connected to the pipeline between the waste liquid tank and the sample tank, one interface of the third three-way valve is used for connecting the pipeline communicated with the waste liquid tank, the other interface is used for connecting the pipeline communicated with the sample tank, and the last interface is used for connecting the branch pipe communicated with the bottom of the separation column and the decay tank.
The third three-way valve is connected to the pipeline between the waste liquid tank and the sample tank, so that the liquid flowing out of the separation column can enter the waste liquid tank after passing through the third three-way valve, and can enter the sample tank through the third three-way valve.
Further, two branch pipes are arranged on the branch pipe, one branch pipe is used for connecting a separation column, and the other branch pipe is used for connecting a decay tank; and the joint of the branch pipe and the branch pipe of the separation column is connected with the decay tank by using a fifth three-way valve.
The fifth three-way valve is connected to the pipeline between the bottom of the separation column and the decay tank, so that the liquid flowing out of the separation column can enter the decay tank after passing through the fifth three-way valve, and can enter the waste liquid tank through the fifth three-way valve.
Further, a fourth three-way valve is connected to the pipeline connecting the target material dissolving tank and the injection pump, one interface of the fourth three-way valve is used for connecting the pipeline communicated with the target material dissolving tank, the other interface is used for connecting the pipeline communicated with the decay tank, and the last interface is used for connecting the pipeline communicated with the injection pump.
The fourth three-way valve is connected to the junction of the discharge pipeline of the target material dissolving tank and the discharge pipeline of the decay tank, and the main pipeline is connected to the injection pump through the fourth three-way valve, so that liquid in the target material dissolving tank and the decay tank can be introduced into the injection pump through the main pipeline connected with the injection pump, and the installation quantity of the pipeline is reduced through the connection of the fourth three-way valve.
Further, the sample tank is connected with a split charging box, and the split charging box is positioned in the shielding box body.
Further, a filter is connected to a pipe connecting the target dissolution tank and the syringe pump.
According to the invention, the filter is connected to the pipeline connecting the target material dissolving tank and the injection pump, so that the target dissolving liquid can be filtered and then enters the separation column, solid particles in the dissolving liquid can be removed, and the device is prevented from being blocked.
Wherein the lining material of the target material dissolving tank adopts polyether-ether-ketone material.
Further, the inner diameter of the separation column is 3-10 mm, and the filler is amide clamp ether type extraction resin with the particle diameter of 50-200 mu m.
The filler in the separation column is limited to the amide-clip ether type extraction resin with the particle size of 50-200 mu m, and the resin has good adsorption capacity to rare earth, and is matched with an automatic control structure in a device, so that the device has large-scale production 47 Ability of Sc.
In another aspect, the present application provides a method of irradiation enrichment from a reactor 46 Extracting Ca target material 47 The Sc method adopts the device to extract;
the method comprises the following steps:
step one: loading the solution into a separation column through a syringe pump, and transferring the effluent into a decay tank for decay;
step two: leaching, namely enabling 5mL of hydrochloric acid to flow through the separation column by using a constant flow pump, transferring the effluent into a decay tank, continuously leaching 10mL of the effluent, and transferring the effluent into a waste liquid tank;
step three, eluting, namely adding a certain volume of hydrochloric acid into the separation column through a constant flow pump, and adsorbing the hydrochloric acid on the separation column 47 Eluting Sc;
step four: occurs in a decay tank 47 Repeating the above steps after standing Ca solution for 3 days for multiple times 47 And Sc extraction.
Enrichment from reactor irradiation using the method described above 46 Extracting Ca target material 47 At Sc, the flow rate of injection is controlled to be 0.1mL/min to 2mL/min when the radioactive solution is transferred by using a syringe pump. The constant flow pump is connected with the eluent storage tank and is used for transferring non-discharged solution, so that isolation between radioactive operations can be effectively realized, and the flow rate controlled by the constant flow pump during transferring the non-discharged solution is 0.1-2 mL/min.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) Enrichment from reactor irradiation in the present invention 46 Extracting Ca target material 47 Sc device can realize the function similar to the generator and improve 47 The yield of Sc has certain degree of automation, can reduce personnel misoperation and irradiation dose, and can obtain high-quality scandium chloride through the device 47 Sc) solution for providing raw materials for nuclear medicine research and development personnel in China for 47 Sc-marked compound and biological experimental study 47 The pace of research and development of Sc-marked medicaments improves the innovation capability of medical isotopes in China;
(2) According to the invention, the filter is connected to the pipeline connecting the target material dissolving tank and the injection pump, so that the dissolved liquid can be filtered and then enters the separation column, and part of impurities in the dissolved liquid can be removed preferentially;
(3) The filler in the separation column is limited to the amide-clip ether type extraction resin with the particle size of 50-200 mu m, and the resin has good adsorption capacity to rare earth, and is matched with an automatic control structure in a device, so that the device has large-scale production 47 Ability of Sc;
(4) The extraction method of the invention is simple and practical, the radioactive operation is simple, the amount of the generated radioactive waste liquid is small, the harm to the body of staff is reduced, the pollution to the environment is also reduced, and 47 the Sc product has high yield and very stable performance.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the drawings that are needed in the examples will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and that other related drawings may be obtained from these drawings without inventive effort for a person skilled in the art. In the drawings:
FIG. 1 shows enrichment from reactor irradiation in accordance with the present invention 46 Extracting Ca target material 47 A schematic structural diagram of the Sc device;
fig. 2 is a flowchart of the present invention when effect verification is performed.
FIG. 3 shows the final result of the present invention 47 Gamma energy spectra of Sc samples.
In the drawings, the reference numerals and corresponding part names:
01-shielding box body, 02-target material dissolving tank, 03-remote controller, 04-leaching/dissolving liquid storage tank, 05-constant flow pump, 06-eluent storage tank, 07-first three-way valve, 08-separation column, 09-separate packing box, 10-second three-way valve, 11-liquid to be recovered, 12-injection pump, 13-sample tank, 14-third three-way valve, 15-waste liquid tank, 16-fourth three-way valve, 17-decay tank and 18-fifth three-way valve.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that: no such specific details are necessary to practice the invention. In other instances, well-known materials or methods have not been described in detail in order to avoid obscuring the present invention.
Throughout the specification, references to "one embodiment," "an embodiment," "one example," or "an example" mean: a particular feature, structure, or characteristic described in connection with the embodiment or example is included within at least one embodiment of the invention. Thus, the appearances of the phrases "in one embodiment," "in an example," or "in an example" in various places throughout this specification are not necessarily all referring to the same embodiment or example. Furthermore, the particular features, structures, or characteristics may be combined in any suitable combination and/or sub-combination in one or more embodiments or examples. Moreover, those of ordinary skill in the art will appreciate that the illustrations provided herein are for illustrative purposes and that the illustrations are not necessarily drawn to scale. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Thus, the following detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in fig. 1, this embodiment provides an enrichment from reactor irradiation 46 Extracting Ca target material 47 Apparatus and methods for Sc. Wherein the structure of the device comprises a screenThe shielding box body 01 is internally provided with a target material dissolving tank 02, a decay tank 17, a waste liquid tank 15, a sample tank 13, a separation column 08, a split charging box 09, a liquid tank to be recovered and an injection pump 12;
the decay tank 17, the waste liquid tank 15 and the sample tank 13 are communicated with the separation column 08;
the separation column 08, the target material dissolving tank 02, the decay tank 17 and the liquid tank 11 to be recovered are all communicated with the injection pump 10;
the syringe pump 10 has the functions of liquid suction and liquid discharge;
the three-way valve is an electromagnetic three-way valve;
the shielding box body 01 is externally connected with a constant flow pump 05 which is communicated with the target material dissolving tank 02 and the separation column 08, and the constant flow pump 05 is connected with a leaching/dissolving liquid storage tank 04 and an eluent storage tank 06 through a conveying pipeline.
The shielding box body 01 is externally connected with a remote controller 03 connected with a constant flow pump 05, an injection pump 12 and an electromagnetic three-way valve;
all the pipes involved in the device were Polyetheretherketone (PEEK) pipes. The polyether-ether-ketone has excellent chemical stability, can resist all strong acid, strong alkali and strong oxidant, does not react with various organic solvents, and has good irradiation resistance. Therefore, the polyether-ether-ketone tube is used, so that the service life of the tube is longer, and new impurities are avoided from being generated due to the action of the extraction material and the tube in the extraction process.
In the device, the target material dissolving tank 02 is used for dissolving the irradiated calcium carbonate target material, and high-concentration hydrochloric acid in the leaching/dissolving liquid storage tank 04 can be selectively introduced into the target material dissolving tank 02 by the constant flow pump 05 for dissolving the calcium carbonate target material; filtering the target solution in the target material dissolving tank 02, and introducing the filtered target solution into the separation column 08 by the injection pump 12 47 Ca/ 47 Sc separation; in the leaching/dissolving liquid storage tank 04, high-concentration hydrochloric acid can be used for leaching and removing redundant calcium by introducing the high-concentration hydrochloric acid into the separation column 08 through the constant flow pump 05 besides being used for dissolving target materials; the eluent storage tank 06 is used for storing low-concentration hydrochloric acid and is introduced into the separation column 08 by the constant flow pump 05 for carrying out 47 Eluting Sc; after a certain period of time, the substance in the decay tank 17 decaysThe syringe pump 12 is passed into the separation column 08 for re-extraction.
Specifically, a first three-way valve 07 is connected to a pipeline connected between the top of the separation column 08 and the constant flow pump 05, one interface of the first three-way valve 07 is used for connecting a pipeline communicated with the constant flow pump 05, the other interface is used for connecting a pipeline communicated with the separation column 08, and the last interface is used for connecting a branch pipe communicated with the injection pump 12 and the liquid tank 11 to be recovered.
A first three-way valve 07 is connected to a pipeline between the top of the separation column 08 and the constant flow pump 05, namely, the first three-way valve 07 can be adjusted, so that the liquid flowing out of the constant flow pump 05 can enter the separation column 08 after passing through the first three-way valve 07, and meanwhile, the liquid can be injected into the separation column 08 through the injection pump 12.
Specifically, the branch pipe is provided with two branch pipes, one branch pipe is used for being connected with the liquid tank 11 to be recovered, the other branch pipe is used for being connected with the injection pump 12, and the branch pipe joint of the liquid tank 11 to be recovered are connected with the injection pump 12 through the second three-way valve 10.
The second three-way valve is connected to the pipeline between the top of the separation column 08 and the liquid tank to be recovered, so that the liquid flowing out of the injection pump can enter the separation column after passing through the second three-way valve, and meanwhile, the liquid can be injected into the liquid tank to be recovered through the injection pump.
Specifically, a third three-way valve 14 is connected to the pipeline between the waste liquid tank 15 and the sample tank 13, one interface of the third three-way valve 14 is used for connecting the pipeline communicated with the waste liquid tank 15, the other interface is used for connecting the pipeline communicated with the sample tank 13, and the last interface is used for connecting the branch pipe communicated with the bottom of the separation column 08 and the decay tank 17.
A third three-way valve 14 is connected to the pipe between the waste liquid tank 15 and the sample tank 13, and the third three-way valve 14 can be adjusted so that the liquid flowing out of the separation column 08 can pass through the third three-way valve 14 and then enter the waste liquid tank 15, and can also enter the sample tank 13 through the third three-way valve 14.
Specifically, two branch pipes are arranged on the branch pipe, one branch pipe is used for being connected with the separation column 08, and the other branch pipe is used for being connected with the decay tank 17; the junction of the branch pipe and the branch pipe connecting the separation column 08 is connected to the decay tank 17 using a fifth three-way valve 18.
A fifth three-way valve 18 is connected to the line between the bottom of the separation column 08 and the decay tank 17, i.e. by adjusting the fifth three-way valve 18, the liquid flowing out of the separation column 08 can pass through the fifth three-way valve 18 and then into the decay tank 17, and can also pass through the fifth three-way valve 18 into the waste liquid tank 15.
Specifically, a fourth three-way valve 16 is connected to the pipeline connecting the target material dissolving tank 02 and the injection pump 12, one interface of the fourth three-way valve 16 is used for connecting the pipeline communicated with the target material dissolving tank 02, the other interface is used for connecting the pipeline communicated with the decay tank 17, and the last interface is used for connecting the pipeline communicated with the injection pump 12.
The junction of the discharging pipeline of the target material dissolving tank 02 and the discharging pipeline of the decay tank 17 is connected with a fourth three-way valve 16, and a main pipeline is connected to the injection pump 12 through the fourth three-way valve 16, so that liquid in the target material dissolving tank 02 and liquid in the decay tank 17 can be introduced into the injection pump 12 through the main pipeline connected with the injection pump 12, and the installation quantity of the pipeline is reduced through the connection of the fourth three-way valve 16.
Specifically, the sample tank 13 is connected with a split charging box 09, and the split charging box 09 is located in the shielding box 01.
Specifically, the inner diameter of the separation column 08 is 5.7mm, and the filler is amide clamp ether type extraction resin with the particle size of 50-100 mu m.
Enrichment from reactor irradiation using the apparatus described above, as shown in FIG. 2 46 Extracting Ca target material 47 Sc performs effect verification.
First, a sample was prepared.
S1: and (3) reactor irradiation: weighing 400mg of natural calcium carbonate, drying, filling into a quartz tube, sealing, welding the quartz tube into an aluminum outer target tube to prepare a target piece, performing helium mass spectrum leak detection, and obtaining a thermal neutron fluence rate of 2 multiplied by 10 14 n·cm -2 s -1 Under irradiation conditionsAfter finishing irradiation, cutting the target piece and taking out the quartz tube after 5 days;
s2: and (3) target material treatment: and cleaning the quartz tube with dilute nitric acid, crushing the head, and pouring out the target material in the quartz tube.
Extraction from the prepared samples using the apparatus described above 47 The Sc method comprises the following steps:
s3: pouring the target material into a target material dissolving tank 02, and dissolving by 3M hydrochloric acid in a leaching/dissolving storage tank to obtain target dissolving liquid;
s4: loading the solution into a column, filtering the solution, adding the solution into a separation column 08 by a syringe pump 12, and transferring the effluent into a decay tank 17 for temporary storage;
s5: leaching, namely 5mL of 3M hydrochloric acid enters a separation column 08 from a leaching/dissolving solution storage tank 04 through a constant flow pump 05, and an effluent is transferred into a decay tank 17; continuously leaching 10mL of 3M hydrochloric acid, and transferring the effluent into a waste liquid tank 15;
s5: eluting, introducing 5mL of 0.1M hydrochloric acid into the separation column 08 via the constant flow pump 05, and adsorbing on the separation column 08 47 Sc elution, and transferring effluent liquid into a sample tank 13;
s6: subpackaging, namely subpackaging the solution in the sample tank 13 into penicillin bottles according to a certain volume through a subpackaging box;
s7: extracting for multiple times: after 3 days of storage of the liquid in decay tank 17, the next time starts 47 Sc extraction is repeated for a plurality of times. .
S8: transferring the solution to be recovered: after the extraction is stopped, the dissolution liquid in the decay tank 17 is transferred to the liquid tank 11 to be recovered by the syringe pump 12.
The detection method comprises the following steps: 1. 47 sc yield is the final scandium chloride 47 Sc) solution in 47 Sc total activity is in the target dissolution liquid 47 The ratio of the total activity of Sc, 47 the activity of Sc was determined by using a high purity germanium gamma spectrometer with a multichannel pulse analyzer (MCA), 47 the activity of Sc was quantified by a gamma ray peak of 159keV (68%).
2、 47 Purity of Sc radionuclides
47 Sc radionuclides purity refers to the purity of the product 47 The percentage of Sc radioactivity in the total radioactivity in the product solution was determined by using a high purity germanium gamma spectrometer with a multichannel pulse analyzer (MCA), where present 46 Sc、 48 Sc and 47 the levels of Ca impurities were determined by measuring gamma ray peaks of 1120.5keV (99.9%), 983.5keV (100.1%) and 1297keV (67%), respectively.
3、 47 Purity of Sc radiochemistry
47 The radiochemical purity of Sc means trivalent 47 Sc 3+ The radioactivity in the form is in the sample 47 Percentage of Sc total radioactivity. Determination by paper chromatography 47 ScCl 3 Solution radiochemical purity, 10. Mu.L was obtained by pipetting with a pipette using physiological saline and 10mmol/L DTPA solution as developing agents, respectively 47 ScCl 3 The sample point is placed on the origin of chromatographic paper (stationary phase), immediately after sample application, the sample point is placed in a chromatographic cylinder containing a developing agent (mobile phase), the liquid level of the developing agent is about 0.5cm lower than the origin, the mobile phase solvent of the developing agent is developed to a certain length (9-10 cm), then the chromatographic paper is taken out, dried, cut into a plurality of sections from the origin to the front edge at equal distance, and each paper section is measured by a high-purity germanium gamma spectrometer 47 Sc activity.
Detection result:
as shown in FIG. 3, the target dissolution solution and the product solution in example 1 were subjected to detection analysis before and after separation 47 Sc activities were 2.12X10 respectively 6 Bq and 1.86×10 6 Bq， 47 The Sc yield is 87.7%, the product index is detected, the radionuclides purity is more than 99.99%, wherein 47 Ca accounts for less than 0.01%, the radiochemical purity is more than 98%, and the contents of metal impurities Al, fe and Pb are less than 0.001 mug/mL.
Example 2
Based on example 1, this example provides an enrichment from reactor irradiation 46 Extracting Ca target material 47 Apparatus and methods for Sc. Unlike example 1, the separation column 08 in this example had an inner diameter of 8.9mm, and other technical features were exactly the same as example 1.
Using the extraction device in this embodiment, adopt andexample 1 the same extraction procedure enriches the extraction apparatus from reactor irradiation 46 Extracting Ca target material 47 Sc performs effect verification. For the same test as in example 1 47 Sc is detected.
Detection result:
the target dissolution solution and the product solution of example 2 were subjected to detection analysis before and after separation 47 Sc activities were 2.36×10 respectively 6 Bq and 1.98X10 6 Bq， 47 The Sc yield is 83.9%, the product index is detected, and the radionuclides purity is more than 99.99%, wherein 47 Ca accounts for less than 0.01%, the radiochemical purity is more than 98%, and the contents of metal impurities Al, fe and Pb are less than 0.001 mug/mL.
Example 3
Based on example 1, this example provides an enrichment from reactor irradiation 46 Extracting Ca target material 47 Apparatus and methods for Sc. Unlike example 1, the packing in the separation column 08 in this example was an amide-clip-ether resin having a particle diameter in the range of 100 to 150 μm, and other technical features were exactly the same as in example 1.
Using the extraction apparatus in this example, the extraction apparatus was enriched from the reactor irradiation using the same extraction method as in example 1 46 Extracting Ca target material 47 Sc performs effect verification. For the same test as in example 1 47 Sc is detected.
The target dissolution solution and the product solution of example 3 were subjected to detection analysis before and after separation 47 Sc activities were 2.09×10, respectively 6 Bq and 1.82×10 6 Bq， 47 The Sc yield is 87.1 percent, the product index is detected, and the radionuclides purity is more than 99.99 percent, wherein 47 Ca accounts for less than 0.01%, the radiochemical purity is more than 98%, and the contents of metal impurities Al, fe and Pb are less than 0.001 mug/mL.
Example 4
Based on example 1, this example provides an enrichment from reactor irradiation 46 Extracting Ca target material 47 Apparatus and methods for Sc. Unlike example 1, the target used for irradiation in this exampleThe feed was 100mg with an enrichment of 5.2% 46 CaCO 3 Other technical features are exactly the same as those of embodiment 1.
Using the extraction apparatus in this example, the extraction apparatus was enriched from the reactor irradiation using the same extraction method as in example 1 46 Extracting Ca target material 47 Sc performs effect verification. For the same test as in example 1 47 Sc is detected.
The target dissolution solution and the product solution of example 4 were subjected to detection analysis before and after separation 47 Sc activities were 6.66×10 respectively 8 Bq and 5.88X10 8 Bq， 47 The Sc yield is 88.3%, the product index is detected, and the radionuclides purity is more than 99.99%, wherein 47 Ca accounts for less than 0.01%, the radiochemical purity is more than 98%, and the contents of metal impurities Al, fe and Pb are less than 0.001 mug/mL.
Example 5
Based on example 1, this example provides an enrichment from reactor irradiation 46 Extracting Ca target material 47 Apparatus and methods for Sc. In this example, the irradiation used a target material of 24.8% enrichment of 100mg, unlike example 1 46 CaCO 3 Other technical features are exactly the same as those of embodiment 1.
Using the extraction apparatus in this example, the extraction apparatus was enriched from the reactor irradiation using the same extraction method as in example 1 46 Extracting Ca target material 47 Sc performs effect verification. For the same test as in example 1 47 Sc is detected.
The target dissolution solution and the product solution of example 5 were subjected to detection analysis before and after separation 47 Sc activities were 3.55X10 respectively 9 Bq and 3.15X10 9 Bq， 47 The Sc yield is 88.7%, the product index is detected, and the radionuclides purity is more than 99.99%, wherein 47 Ca accounts for less than 0.01%, the radiochemical purity is more than 98%, and the contents of metal impurities Al, fe and Pb are less than 0.001 mug/mL.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (11)
1. Enrichment from reactor irradiation 46 Extracting Ca target material 47 The Sc device is characterized by comprising a shielding box body (01), wherein a target material dissolving tank (02), a decay tank (17), a waste liquid tank (15), a sample tank (13), a separation column (08), an injection pump (12), a split charging box (09) and a liquid tank (11) to be recovered are arranged in the shielding box body (01);
the decay tank (17), the waste liquid tank (15) and the sample tank (13) are communicated with the separation column (08) through a third three-way valve (14) and a fifth three-way valve (18);
the separation column (08), the target material dissolving tank (02), the decay tank (17) and the liquid tank (11) to be recovered are communicated with the injection pump (12) through a first three-way valve (07), a second three-way valve (10) and a fourth three-way valve (16);
the injection pump (12) has the functions of liquid suction and liquid discharge,
the first three-way valve (07), the second three-way valve (10), the third three-way valve (14), the fourth three-way valve (16) and the fifth three-way valve (18) are all electromagnetic three-way valves;
the shielding box body (01) is externally connected with a constant flow pump (05) communicated with the target material dissolving tank (02) and the separation column (08), and the constant flow pump (05) is connected with a leaching/dissolving liquid storage tank (04) and an eluent storage tank (06) through a conveying pipeline;
the shielding box body (01) is externally connected with a remote controller (03) which is in communication connection with the constant flow pump (05), the injection pump (12) and the electromagnetic three-way valve.
2. Enrichment from reactor irradiation according to claim 1 46 Extracting Ca target material 47 Sc device is characterized in that a first three-way valve (07) is connected on a pipeline connected between the top of the separation column (08) and the constant flow pump (05), the device comprisesOne interface of the first three-way valve (07) is used for connecting a pipeline communicated with the constant flow pump (05), the other interface is used for connecting a pipeline communicated with the separation column (08), and the last interface is used for connecting a branch pipe communicated with the injection pump (12) and the liquid tank (11) to be recovered.
3. Enrichment from reactor irradiation according to claim 2 46 Extracting Ca target material 47 Sc's device, its characterized in that, the branch pipe is provided with two branch pipes, and one of them is used for connecting to wait to retrieve fluid reservoir (11), and another is used for connecting syringe pump (12), connects the branch pipe of waiting to retrieve fluid reservoir (11) and branch pipe junction use second three-way valve to connect syringe pump (12).
4. Enrichment from reactor irradiation according to claim 1 46 Extracting Ca target material 47 Sc's device, its characterized in that is connected with the third three-way valve on the pipeline between waste liquid jar (15) and sample jar (13), one interface of third three-way valve is used for connecting the pipeline with waste liquid jar (15) intercommunication, another interface is used for connecting with the pipeline of sample jar (13) intercommunication, last interface is used for connecting with the branch pipe of separator 08) bottom and decay jar (17) intercommunication.
5. Enrichment from reactor irradiation according to claim 1 46 Extracting Ca target material 47 The Sc device is characterized in that a pipeline connecting the target material dissolving tank (02) and the injection pump (12) is connected with a fourth three-way valve (16), one interface of the fourth three-way valve (16) is used for connecting a pipeline communicated with the target material dissolving tank (02), the other interface is used for connecting a pipeline communicated with the decay tank (17), and the last interface is used for connecting a pipeline communicated with the injection pump (12).
6. Enrichment from reactor irradiation according to claim 4 46 Extracting Ca target material 47 The Sc device is characterized in that the branch pipe is provided with two branch pipesOne of the branch pipes is used for connecting a separation column (08), and the other branch pipe is used for connecting a decay tank (17); the connection of the branch pipe and the branch pipe of the separation column (08) is connected with the decay tank (17) by a fifth three-way valve (18).
7. Enrichment from reactor irradiation according to claim 1 46 Extracting Ca target material 47 Sc, characterized in that, the sample tank (13) is connected with a split charging box (09), and the split charging box (09) is located in the shielding box body (01).
8. Enrichment from reactor irradiation according to claim 1 46 Extracting Ca target material 47 The Sc device is characterized in that a filter is connected to a pipeline connecting the target material dissolving tank (02) and the injection pump (12).
9. Enrichment from reactor irradiation according to claim 1 46 Extracting Ca target material 47 The Sc device is characterized in that the inner diameter of the separation column (08) is 3-10 mm, and the filler is amide clamp ether type extraction resin with the particle size of 50-200 mu m.
10. Enrichment from reactor irradiation 46 Extracting Ca target material 47 A method of Sc, characterized in that extraction is carried out by means of the device according to any one of claims 1 to 9.
11. Enrichment from reactor irradiation according to claim 10 46 Extracting Ca target material 47 A method of Sc comprising the steps of:
step one: loading the solution into a separation column (08) through a syringe pump (12), and transferring the effluent into a decay tank (17) for decay;
step two: leaching, namely enabling 5mL of hydrochloric acid to flow through the separation column (08) by using a constant flow pump (05), transferring the effluent into a decay tank (17), continuously leaching 10mL, and transferring the effluent into a waste liquid tank (15);
step three, the step three is that,eluting, adding a certain volume of hydrochloric acid into the separation column (08) by a constant flow pump (05), and adsorbing on the separation column (08) 47 Eluting Sc;
step four: takes place, the decay tank (17) contains 47 Standing Ca solution for 3 days, repeating the above steps for multiple times 47 And Sc extraction.
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