CN117604283A - A slave 227 Ac- 223 Recovery from Ra generators 227 Ac method - Google Patents
A slave 227 Ac- 223 Recovery from Ra generators 227 Ac method Download PDFInfo
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- CN117604283A CN117604283A CN202311593599.XA CN202311593599A CN117604283A CN 117604283 A CN117604283 A CN 117604283A CN 202311593599 A CN202311593599 A CN 202311593599A CN 117604283 A CN117604283 A CN 117604283A
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- 238000011084 recovery Methods 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000000926 separation method Methods 0.000 claims abstract description 50
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 41
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 230000000737 periodic effect Effects 0.000 claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 claims abstract description 8
- 239000012141 concentrate Substances 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 68
- 238000002386 leaching Methods 0.000 claims description 25
- 239000003480 eluent Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 20
- 239000007790 solid phase Substances 0.000 claims description 18
- 238000010828 elution Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 10
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000003456 ion exchange resin Substances 0.000 claims description 9
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 230000000717 retained effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 230000001954 sterilising effect Effects 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims 1
- 229910052500 inorganic mineral Inorganic materials 0.000 claims 1
- 239000011707 mineral Substances 0.000 claims 1
- 150000007524 organic acids Chemical class 0.000 claims 1
- 239000008215 water for injection Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000004440 column chromatography Methods 0.000 abstract description 8
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 3
- 239000002910 solid waste Substances 0.000 abstract description 3
- 238000009270 solid waste treatment Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 11
- 239000011147 inorganic material Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 9
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 8
- 238000004064 recycling Methods 0.000 description 7
- 238000012544 monitoring process Methods 0.000 description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 239000007822 coupling agent Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012217 radiopharmaceutical Substances 0.000 description 4
- 229940121896 radiopharmaceutical Drugs 0.000 description 4
- 230000002799 radiopharmaceutical effect Effects 0.000 description 4
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 206010028980 Neoplasm Diseases 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- -1 acyl chlorinated di (2-ethylhexyl) phosphate Chemical class 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 230000005255 beta decay Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
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- 238000005660 chlorination reaction Methods 0.000 description 2
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
- 238000002560 therapeutic procedure Methods 0.000 description 2
- 210000001519 tissue Anatomy 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010027476 Metastases Diseases 0.000 description 1
- 229910006124 SOCl2 Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 229910052767 actinium Inorganic materials 0.000 description 1
- QQINRWTZWGJFDB-UHFFFAOYSA-N actinium atom Chemical compound [Ac] QQINRWTZWGJFDB-UHFFFAOYSA-N 0.000 description 1
- 230000005262 alpha decay Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a slave 227 Ac‑ 223 Recovery from Ra generators 227 The Ac method belongs to the technical field of parent nuclide recovery in the radioisotope production process. The slave provided by the invention 227 Ac‑ 223 In Ra generators 227 Ac recovery method, purifying 227 Ac solution is filled into the separation column 227 Ac adsorption to produce 227 Ac‑ 223 Ra generator, periodic rinsing with low concentration inorganic acid, eluting with high concentration inorganic acid (failure or not), collecting 227 Ac recovery solution, pair 227 Concentrating the Ac recovered solution and regulating acidity to obtain 227 Ac concentrate. The column chromatography separation method of the invention comprises the following operation stepsThe number of the steps is small, the flow is simple, 227 the recovery rate of Ac parent nuclide is high (more than or equal to 98 percent), and the solid waste generated and recovered by the generator is effectively reduced 227 Ac has completed concentration and acidity adjustment, is convenient for reuse, and greatly reduces the preparation 227 The cost of Ac parent nuclide and the cost of solid waste treatment are large-scale production 223 The Ra lays a foundation and promotes the development of medical isotopes and pharmaceutical industry.
Description
Technical Field
The invention relates to the technical field of parent nuclide recovery in the production process of radioactive isotopes, in particular to a secondary method 227 Ac- 223 Recovery from Ra generators 227 Ac method.
Background
Targeted alpha therapy (Targeted alpha therapy, TAT) is a rapidly evolving field that uses alpha radionuclides to selectively deliver a dose of radiation that kills cells to a tumor site, with low penetration range (50-90 μm) and highly linear energy-transferred alpha particles (tens to hundreds of keV/μm) that are able to maximize destruction of cancer cells with minimal damage to surrounding healthy tissue. 223 Ra, the first alpha-targeted therapeutic nuclide approved for clinical treatment, has a physical half-life of 11.4d, emits only alpha rays, and has less radiation damage to normal tissues when it is locally absorbed as a radiopharmaceutical into the human body. Therefore, the method has obvious advantages in the aspect of treating tumor bone metastasis, and is a therapeutic nuclide with important application value.
Several preparations studied at present 223 Among the methods for Ra, the most convenient and common method is to use 227 Ac- 223 Ra generator. In the case of the generator(s), 227 ac beta decay to 227 Th， 227 Th undergoes alpha decay to 223 Ra, can be obtained by separation and purification 223 RaCl 2 A solution. While 227 Ac- 223 One of the key components in Ra generators is the parent nuclide 227 Ac (its product)The physical half-life is 21.77 years). 227 Ac can be obtained by several methods: (1) To be used for 226 Ra is target material, and after the reactor is irradiated, the reaction is carried out 226 Ra(n,γ) 227 Ra generated 227 Ra beta decay to 227 Ac; (2) From the following components 232 Th proton fission production 227 Ac; (3) From 235 U has a very low content due to its natural decay, and one ton of uranium ores contains about one tenth of a gram of actinium. Thus, mass production 227 The most viable method of Ac is also by reactor irradiation 226 Ra is produced.
At the same time 227 Ac- 223 Ra generator preparation 223 In the Ra process, the core separating material is subjected to strong radiation for a long time, so that the separating material is irradiated and degraded in the long-term use process to cause material failure or in the eluent 223 The Ra activity does not satisfy the conditions for use. Due to 227 Ac half-life is 21.77 years and is prepared by irradiation 227 Raw material of Ac 226 Ra extraction is difficult and the source of goods is scarce. If at this time directly contain 227 Ac (alternating current) 227 Ac- 223 The Ra generator is disposed of as waste, which not only results in a large economic loss but also results in a waste of limited raw materials. Thus, to reduce 223 Production cost of Ra is not satisfied 227 Ac- 223 In Ra generators 227 And (5) recycling Ac. And has not been reported at present 227 Recovery method of Ac.
Disclosure of Invention
For the purpose of 227 Ac- 223 The Ra generator has the advantages that after long-term use is found in the early research process, the performance of separation materials of the generator is reduced, the leaching efficiency is reduced, and the Ra generator is obtained 223 RaCl 2 Insufficient activity and the like, and 227 difficulty in obtaining Ac, scarcity of resources, and production 227 Ac is costly and at present 227 The technology of Ac recycling is blank. The present invention aims to provide a slave 227 Ac- 223 Recovery from Ra generators 227 Ac method can be realized by simple column chromatography separation process 227 Recovery of Ac thereby to achieve 227 Recycling of AcPreparation of radiopharmaceuticals with relief 223 RaCl 2 When the parent nuclide is 227 The problem of insufficient Ac resource can achieve the purposes of saving cost and raw materials
The invention is realized by the following technical scheme:
the invention provides a slave 227 Ac- 223 Recovery from Ra generators 227 A method of Ac comprising:
will contain 227 Ac and the solution of decay daughter thereof are transferred as upper column liquid to a separating material filled with phosphate extractant or a separating column of ion exchange resin for contact, 0.005 mol/L-0.5 mol/L of inorganic acid is added for leaching, 227 ac and 227 th is retained in the separation column and is obtained to contain 223 Standing the elution solution of Ra and daughter nuclides to be treated 223 After Ra regenerates a certain amount, continuously using 0.005 mol/L-0.5 mol/L inorganic acid to make periodical and repeated leaching to obtain the invented product containing 223 A first eluent of Ra and its daughter nuclides;
to be treated 223 Drop in Ra leaching efficiency or 223 When the activity of Ra is reduced, adding 1.0 mol/L-10.0 mol/L inorganic acid into the separation column for eluting to obtain a liquid containing 227 Ac、 227 Th、 223 Concentrating the second eluent and regulating the acid system with inorganic acid of 0.005 mol/L-0.5 mol/L to obtain parent body 227 Ac concentrate.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the Ac method, contain 227 Ac and decay daughter thereof 227 The Ac activity is 0.01 mCi-1 Ci.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the Ac method, the period leaching time of the period leaching 223Ra is not less than 1 day/time according to the amount of 227Ac filled.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the method of Ac, the preparation of the separation column comprises the following steps: loading the separation material into a separation column, and sequentially introducingPre-treating and flushing the sterilized injection water and inorganic acid, and adjusting the flow rate to be 0.01-3.0 mL/min;
preferably, the inorganic acid is nitric acid, hydrochloric acid, medical hydrochloric acid, sulfuric acid or perchloric acid.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the method of Ac, the inorganic acid used for periodic repeated leaching or the inorganic acid used for elution comprises the following steps: nitric acid, hydrochloric acid, medical hydrochloric acid, sulfuric acid or perchloric acid;
preferably, the flow rate of leaching by inorganic acid is 0.01 mL/min-3.0 mL/min;
preferably, the flow rate of elution with an inorganic acid is 0.01mL/min to 5.0mL/min. Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the Ac method, the washing is carried out periodically 223 The inorganic acid used by Ra is medical hydrochloric acid, the acidity is 0.005 mol/L-0.5 mol/L, and the flow rate of the medical hydrochloric acid is 0.01 mL/min-3.0 mL/min;
preferably, elution 227 The inorganic acid used in Ac is medical hydrochloric acid, the acidity is 1.0 mol/L-10.0 mol/L, and the flow rate of the medical hydrochloric acid is 0.01 mL/min-5.0 mL/min.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the method of Ac, the separation column filled phosphate-containing extractant separation material comprises: one or more of P204 extract resin, P507 extract resin, 04 solid phase extractant, P507 solid phase extractant and Cyanex272 extract resin; and
The ion exchange resin packed in the separation column comprises: one or more of Dowex 50WX8, dowex 1X8 and nuclear grade ion exchange resin.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the method of Ac, the second eluent is concentrated by the following steps: reduced pressure distillation, atmospheric distillation, baking or evaporation; when concentrating, the heating temperature is 60-120 ℃, and the heating time is 10-360 min.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the Ac method, the obtained composition contains 227 Ac、 227 Th、 223 The volume of the second eluent of Ra and its daughter nuclides is not less than 5mL.
Further, at the slave 227 Ac- 223 Recovery from Ra generators 227 In the Ac method, the inorganic acid adopted by the acid system is medical hydrochloric acid with the acid concentration not higher than 0.1 mol/L.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the slave provided by the invention 227 Ac- 223 Recovery from Ra generators 227 Ac method can be realized by simple column chromatography separation process 227 Recovery of Ac thereby to achieve 227 Recycling Ac to realize large-scale production 223 Lay foundation for Ra and ease preparation of radiopharmaceuticals 223 RaCl 2 When the parent nuclide is 227 The problem of insufficient Ac resources can achieve the purposes of saving cost and raw materials. The invention adopts a column chromatography separation process to separate from 227 Ac- 223 Recovery from Ra generators 227 Ac, greatly reduces personnel exposure dose and environmental pollution, and reduces 223 Waste treatment costs of Ra production process.
2. The slave provided by the invention 227 Ac- 223 Recovery from Ra generators 227 Ac method, which can recover the residue in the generator separation column 227 Ac, and recycle it, which can alleviate 227 The problem of insufficient Ac raw material can be reduced 223 Production cost of Ra. The treatment process is simple and environment-friendly, and can effectively realize 227 Ac recycling achieves the purposes of saving cost and raw materials, fills up 227 Ac- 223 Recovery from Ra generators 227 The Ac technology is blank, and the preparation and recovery of the radioactive isotope are perfected. The recovery method has simple and practical operation and low economic cost, and is 223 High value for Ra production 227 The recovery of Ac provides an effective solution for large-scale preparation 223 Ra opens up a key technical link.
3. The invention providesFor the slave 227 Ac- 223 Recovery from Ra generators 227 The Ac method uses column chromatography separation, has few operation steps and simple flow, 227 the recovery rate of Ac parent nuclide is high (more than or equal to 98 percent), and the solid waste generated and recovered by the generator is effectively reduced 227 Ac has completed concentration and acidity adjustment, is convenient for reuse, and greatly reduces the preparation 227 The cost of Ac parent nuclide and the cost of solid waste treatment are large-scale production 223 The Ra lays a foundation and promotes the development of medical isotopes and pharmaceutical industry.
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 a slave according to the present invention 227 Ac- 223 Recovery from Ra generators 227 A flow chart of a method of Ac.
Detailed Description
For the purpose of making apparent the objects, technical solutions and advantages of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, wherein the exemplary embodiments of the present invention and the descriptions thereof are for illustrating the present invention only and are not to be construed as limiting the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The technical scheme of the invention is as follows:
referring to FIG. 1, a slave unit is shown 227 Ac- 223 Recovery from Ra generators 227 A method of Ac comprising:
will contain 227 Ac and its decay daughter solution as column loading solution is transferred into a column filled with phosphateThe separation material of the extractant or the separation column of the ion exchange resin is contacted for 0.5 to 2 hours, which can be 0.5 hour, 1 hour, 1.5 hours, 2 hours and other time; adding 0.005 mol/L-0.5 mol/L inorganic acid for leaching, wherein the concentration can be 0.005mol/L, 0.01mol/L, 0.05mol/L, 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L and the like; 227 ac and 227 th is retained in the separation column and is obtained to contain 223 Standing the elution solution of Ra and daughter nuclides to be treated 223 After a certain amount of Ra regenerates, continuously using 0.005 mol/L-0.5 mol/L inorganic acid to carry out periodical and repeated leaching, wherein the concentration can be 0.005mol/L, 0.01mol/L, 0.05mol/L, 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L and the like; obtaining the content of 223 A first eluent of Ra and its daughter nuclides;
to be treated 223 Drop in Ra leaching efficiency or 223 When the activity of Ra is reduced, adding 1.0mol/L to 10.0mol/L of inorganic acid into the separation column for eluting, wherein the concentration can be 1mol/L, 2mol/L, 3mol/L, 4mol/L, 5mol/L, 6mol/L, 7mol/L, 8mol/L, 9mol/L, 10mol/L and the like; obtaining the content of 227 Ac、 227 Th、 223 The second eluent of Ra and daughter nuclides thereof is concentrated and an acid system is regulated by using inorganic acid with the concentration of 0.005mol/L to 0.5mol/L, wherein the concentration can be 0.005mol/L, 0.01mol/L, 0.05mol/L, 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L and the like; obtaining a parent body 227 Ac concentrate.
The slave provided by the invention 227 Ac- 223 Recovery from Ra generators 227 Ac method, purifying 227 Ac solution is filled into the separation column 227 Ac adsorption to produce 227 Ac- 223 Ra generator, periodic rinsing with low concentration inorganic acid, eluting with high concentration inorganic acid (failure or not), collecting 227 Ac recovery solution, pair 227 Concentrating the Ac recovered solution and regulating acidity to obtain 227 Ac concentrate.
The recovery method provided by the invention can be realized through a simple column chromatography separation process 227 Recovery of Ac thereby to achieve 227 Recycling of AcTo realize large-scale production 223 Lay foundation for Ra and ease preparation of radiopharmaceuticals 223 RaCl 2 When the parent nuclide is 227 The problem of insufficient Ac resources can achieve the purposes of saving cost and raw materials. The invention adopts a column chromatography separation process to separate from 227 Ac- 223 Recovery from Ra generators 227 Ac, greatly reduces personnel exposure dose and environmental pollution, and reduces 223 Waste treatment costs of Ra production process.
The recovery method provided by the invention can recover the residue in the generator separation column 227 Ac, and recycle it, which can alleviate 227 The problem of insufficient Ac raw material can be reduced 223 Production cost of Ra. The treatment process is simple and environment-friendly, and can effectively realize 227 Ac recycling achieves the purposes of saving cost and raw materials, fills up 227 Ac- 223 Recovery from Ra generators 227 The Ac technology is blank, and the preparation and recovery of the radioactive isotope are perfected. The recovery method has simple and practical operation and low economic cost, and is 223 High value for Ra production 227 The recovery of Ac provides an effective solution for large-scale preparation 223 Ra opens up a key technical link.
The column chromatography separation method used in the invention has the advantages of few operation steps and simple flow, 227 the recovery rate of Ac parent nuclide is high (more than or equal to 98 percent), and the solid waste generated and recovered by the generator is effectively reduced 227 Ac has completed concentration and acidity adjustment, is convenient for reuse, and greatly reduces the preparation 227 The cost of Ac parent nuclide and the cost of solid waste treatment are large-scale production 223 The Ra lays a foundation, promotes the development of medical isotopes and pharmaceutical industry and helps the implementation of 'health China' strategy.
Further comprises 227 Ac and decay daughter thereof 227 The Ac activity is 0.01mCi to 1Ci, and may be 0.01mCi, 0.05mCi, 0.1mCi, 1mCi, 50mCi, 100mCi, 500mCi, 700mCi, 1000Ci, or the like.
Further, according to the filling 227 The Ac content was varied, weeksStage leaching 223 The period leaching time of Ra is not less than 1 day/time. The period of rinsing can be 1 day/time, one month/time, one time of two months, etc., until the rinsing time for reaching complete equilibrium is about 200 days.
Further, the preparation of the separation column includes: 1 g-4 g of separation material is filled into a separation column, and pretreatment flushing is carried out sequentially through 10 mL-50 mL of sterilization injection water and 10 mL-50 mL of inorganic acid, and the flow rate is regulated to be 0.01 mL/min-3.0 mL/min, and can be 0.01mL/min, 0.05mL/min, 0.1mL/min, 0.5mL/min, 1mL/min, 2mL/min, 3mL/min and other flow rates.
Preferably, the inorganic acid is nitric acid, hydrochloric acid, medical hydrochloric acid, sulfuric acid or perchloric acid.
Further, the inorganic acid used for the periodic repeated elution or the inorganic acid used for the elution includes: nitric acid, hydrochloric acid, medical hydrochloric acid, sulfuric acid or perchloric acid;
preferably, the flow rate of leaching by using inorganic acid is 0.01 mL/min-3.0 mL/min, and the flow rate can be 0.01mL/min, 0.05mL/min, 0.1mL/min, 0.5mL/min, 1mL/min, 2mL/min, 3mL/min and the like;
preferably, the flow rate of elution with an inorganic acid is 0.01mL/min to 5.0mL/min, and may be 0.01mL/min, 0.05mL/min, 0.1mL/min, 0.5mL/min, 1mL/min, 3mL/min, 5mL/min, etc.
Further, periodic rinsing 223 The inorganic acid used by Ra is medical hydrochloric acid, the acidity is 0.005 mol/L-0.5 mol/L, and can be 0.005mol/L, 0.01mol/L, 0.05mol/L, 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L and the like; the flow rate of the medical hydrochloric acid is 0.01-5.0 mL/min, and can be 0.01mL/min, 0.05mL/min, 0.1mL/min, 0.5mL/min, 1mL/min, 3mL/min, 5mL/min and other flow rates.
Preferably, elution 227 The inorganic acid used in Ac is medical hydrochloric acid, the acidity is 1.0 mol/L-10.0 mol/L, and can be 1mol/L, 2mol/L, 3mol/L, 4mol/L, 5mol/L, 6mol/L, 7mol/L, 8mol/L, 9mol/L, 10mol/L and other acidity; the flow rate of the medical hydrochloric acid is 0.01 mL/min-5.0 mL/min, and the flow rates can be 0.01mL/min, 0.05mL/min, 0.1mL/min, 0.5mL/min, 1mL/min, 3mL/min, 5mL/min and the like. Feeding inIn one step, the separation column packed phosphate-containing extractant separation material comprises: one or more of P204 extract resin, P507 extract resin, P204 solid phase extractant, P507 solid phase extractant and Cyanex272 extract resin; and
The ion exchange resin packed in the separation column comprises: one or more of Dowex 50WX8, dowex 1X8 and nuclear grade ion exchange resin. Wherein, the P204 extraction resin and the P507 extraction resin are commercial existing substances; the P507 solid phase extractant and the P204 solid phase extractant are self-made solid phase extractants, preferably self-made solid phase extractants, have the advantages of strong mechanical property and good irradiation resistance, and can be better suitable for separating nuclear radioactive substances.
The preparation method of the self-made P204 solid phase extractant comprises the following steps:
step S1, performing acyl chlorination on di (2-ethylhexyl) phosphate to obtain acyl chlorinated di (2-ethylhexyl) phosphate;
mixing di (2-ethylhexyl) phosphate with thionyl chloride and pyridine, and then adding the mixture into an organic solvent for heating reflux to obtain acyl chlorinated di (2-ethylhexyl) phosphate;
s2, grafting an inorganic material by adopting a silane coupling agent to obtain an inorganic material grafted with the coupling agent, wherein the inorganic material is an inorganic material with hydroxyl on the surface;
and S3, grafting the acyl-chlorinated di (2-ethylhexyl) phosphate obtained in the step S1 on the inorganic material of the grafting coupling agent obtained in the step S2 to obtain the solid-phase extracting agent.
The preparation method of the self-made P507 solid phase extractant comprises the following steps:
step S1, carrying out acyl chlorination on 2-ethylhexyl phosphate mono-2-ethylhexyl ester to obtain acyl chlorinated 2-ethylhexyl phosphate mono-2-ethylhexyl ester;
mixing 2-ethylhexyl phosphate mono-2-ethylhexyl ester with metal sodium, adding into a solvent of a machine, heating and refluxing to obtain saponified 2-ethylhexyl phosphate mono-2-ethylhexyl ester, adding SOCl2 and pyridine, and refluxing to obtain acyl-chlorinated 2-ethylhexyl phosphate mono-2-ethylhexyl ester;
s2, grafting an inorganic material by adopting a silane coupling agent to obtain an inorganic material grafted with the coupling agent, wherein the inorganic material is an inorganic material with hydroxyl on the surface;
and S3, grafting the 2-ethylhexyl phosphate mono-2-ethylhexyl ester obtained in the step S1 on the inorganic material of the grafting coupling agent obtained in the step S2 to obtain the solid-phase extracting agent.
Wherein the silane coupling agent comprises 3-aminopropyl triethoxysilane; inorganic materials include silica, zirconia, alumina or titania.
Further, the second eluent is concentrated in a manner comprising: reduced pressure distillation, atmospheric distillation, baking or evaporation; when concentrating, the heating temperature is 60-120 ℃, which can be 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃ or 120 ℃, etc.; the heating time is 10 min-360 min, and can be 10min, 60min, 120min, 180min, 240min, 300min, 360min, etc.
Further, obtain the product containing 227 Ac、 227 Th、 223 The volume of the second eluent of Ra and its daughter nuclides is not less than 5mL.
Further, the inorganic acid adopted by the acid system is medical hydrochloric acid with the acid concentration not higher than 0.1 mol/L.
The invention is equally applicable to compositions comprising 227 The Ac solution can be separated and purified by directly using a separating material P204 solid phase extractant 227 Separating and purifying Ac.
The invention is equally applicable to compositions containing only 227 Ac and its mother liquor of decay daughter can be directly carried out by using P204 solid phase extractant 227 Ac、 227 Th and 223 isolation of Ra.
To further illustrate the invention, the following provides a slave according to the invention in connection with the examples 227 Ac- 223 In Ra generators 227 The Ac recovery process is described, but it should be understood that these examples are presented with the understanding that the present invention is to be practiced with the help of specific embodiments and specific procedures, and that these are merely to further illustrate the features and aspects of the present inventionAdvantages, and not limitations, are set forth in the claims, nor are the scope of the invention limited by the examples which follow.
Example 1
Two 2g portions of P204 solid phase extractant are weighed and respectively put into a separation column 1# and a separation column 2# with the inner diameter of 10mm and the height of 80mm, 30mL of sterilization injection water and 30mL of medical hydrochloric acid with the mol/L of 0.005 are respectively used for pretreatment of the separation column, and the flow rate is regulated to be 0.8mL/min.
Example 2
Two 4mCi (about 2 mL) purified portions were taken 227 The Ac solution was used as the column loading solution. At room temperature, the solution is filled into the separation column 1# and the separation column 2# in the example 1 at a flow rate of 0.6mL/min by a pump, and after the column-filling solution A is contacted with the P204 solid phase extractant for 0.5h, the solution is rinsed at a flow rate of 0.1mL/min by adding 0.005mol/L of medical hydrochloric acid. After leaching 10mL 223 Collecting Ra (about 1.1 mCi) to obtain colorless transparent eluate, wherein 227 Ac and 227 th is completely retained in the separation column. Standing for a week 223 After Ra regenerates a certain amount, the leaching process is continuously repeated by using medical hydrochloric acid with the concentration of 0.005mol/L (the step is carried out periodically), thus obtaining the product containing 223 Colorless transparent leacheate of Ra and daughter nuclides thereof can be obtained by leaching each time 223 The amount of Ra was about 1.3mCi.
Example 3
After the separation column 1# in example 2 was used for 6 months [ ] 223 Ra separation efficiency, elution efficiency and activity are not obviously changed), 5.0mol/L medical hydrochloric acid is added into a separation column at room temperature to carry out elution at a flow rate of 1.0mL/min, eluent is collected at 1.0 mL/part, total 15mL is collected, and eluent II (containing 227 Ac、 227 Th、 223 Ra and daughter nuclides) for continuous monitoring of daughter nuclides by 227 Calculated and recovered Th increment 227 Ac, monitoring found the first 8mL 227 The Th is obviously increased, and 3.4mCi is obtained through calculation and recovery 227 Ac, then 7mL of eluent was not found during the monitoring 227 Th increases. The results indicate recovery 227 Ac mainConcentrate on the first 8.0mL.
Example 4
After the failure of the separation column # 2 in example 2 223 Ra separation efficiency, leaching efficiency and activity are obviously changed), 8.0mol/L medical hydrochloric acid is added into a separation column at room temperature to carry out leaching at a flow rate of 0.3mL/min, eluent is collected at 1.0 mL/part, 15mL is collected in total, daughter nuclide continuous monitoring is carried out on the eluent obtained by collection, and the method comprises the steps of 227 Calculated and recovered Th increment 227 Ac, monitoring found 9mL before 227 The Th is obviously increased, and 2.8mCi is obtained through calculation and recovery 227 Ac, then 6mL of eluent was not found during the monitoring 227 Th increases. The results indicate recovery 227 Ac was mainly concentrated in the first 9.0mL.
Example 5
Heating and concentrating the eluent in example 3 or example 4 at 90deg.C in a shielding box to near dryness, dissolving with 0.005mol/L medical hydrochloric acid, repeating for more than 3 times, and adjusting acid system to 0.005mol/L medical hydrochloric acid to obtain parent nuclide 227 Ac concentrate.
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 (10)
1. A slave 227 Ac- 223 Recovery from Ra generators 227 A method of Ac comprising:
will contain 227 Ac and the solution of decay daughter thereof are transferred as upper column liquid to a separating material filled with phosphate extractant or a separating column of ion exchange resin for contact, 0.005 mol/L-0.5 mol/L of inorganic acid is added for leaching, 227 ac and 227 th is retained in the separation column and is obtained to contain 223 Ra and its seedStanding the eluent of the nuclide to be treated 223 After Ra regenerates a certain amount, continuously using 0.005 mol/L-0.5 mol/L inorganic acid to make periodical and repeated leaching to obtain the invented product containing 223 A first eluent of Ra and its daughter nuclides;
to be treated 223 Drop in Ra leaching efficiency or 223 When the activity of Ra is reduced, adding 1.0 mol/L-10.0 mol/L inorganic acid into the separation column for eluting to obtain a liquid containing 227 Ac、 227 Th、 223 Concentrating the second eluent and regulating the acid system with inorganic acid of 0.005 mol/L-0.5 mol/L to obtain parent body 227 Ac concentrate.
2. The slave according to claim 1 227 Ac- 223 Recovery from Ra generators 227 A method of Ac, characterized by comprising 227 Ac and decay daughter thereof 227 The Ac activity is 0.01 mCi-1 Ci.
3. The slave according to claim 1 227 Ac- 223 In Ra generators 227 A method for recovering Ac, characterized in that, according to the filling 227 Ac in different amounts, periodic leaching 223 The period of Ra is not less than 1 day.
4. The slave according to claim 1 227 Ac- 223 Recovery from Ra generators 227 A method of Ac, characterized in that the preparation of the separation column comprises: loading the separation material into a separation column, sequentially carrying out pretreatment flushing by sterilizing water for injection and inorganic acid, and regulating the flow rate to be 0.01-3.0 mL/min;
preferably, the inorganic acid is nitric acid, hydrochloric acid, medical hydrochloric acid, sulfuric acid or perchloric acid.
5. The slave according to claim 1 227 Ac- 223 Recovery from Ra generators 227 Ac method, characterized in that the mineral acid used for periodic repeated leaching or the absence of elution is usedThe organic acid comprises: nitric acid, hydrochloric acid, medical hydrochloric acid, sulfuric acid or perchloric acid;
preferably, the flow rate of leaching by inorganic acid is 0.01 mL/min-3.0 mL/min;
preferably, the flow rate of elution with an inorganic acid is 0.01mL/min to 5.0mL/min.
6. The slave according to claim 5 227 Ac- 223 Recovery from Ra generators 227 Ac method, characterized in that it comprises periodic rinsing 223 The inorganic acid used by Ra is medical hydrochloric acid, the acidity is 0.005 mol/L-0.5 mol/L, and the flow rate of the medical hydrochloric acid is 0.01 mL/min-3.0 mL/min;
preferably, elution 227 The inorganic acid used in Ac is medical hydrochloric acid, the acidity is 1.0 mol/L-10.0 mol/L, and the flow rate of the medical hydrochloric acid is 0.01 mL/min-5.0 mL/min.
7. The slave according to claim 1 227 Ac- 223 Recovery from Ra generators 227 The Ac method is characterized in that the separating column filled phosphate-containing extractant separating material comprises the following components: one or more of P204 extract resin, P507 extract resin, P204 solid phase extractant, P507 solid phase extractant and Cyanex272 extract resin; and
The ion exchange resin packed in the separation column comprises: one or more of Dowex 50WX8, dowex 1X8 and nuclear grade ion exchange resin.
8. The slave according to claim 1 227 Ac- 223 Recovery from Ra generators 227 A method of Ac, characterized in that the second eluent is concentrated by: reduced pressure distillation, atmospheric distillation, baking or evaporation; when concentrating, the heating temperature is 60-120 ℃, and the heating time is 10-360 min.
9. The slave according to claim 1 227 Ac- 223 Recovery from Ra generators 227 A process for Ac, characterized in that a catalyst containing 227 Ac、 227 Th、 223 The volume of the second eluent of Ra and its daughter nuclides is not less than 5mL.
10. The slave according to claim 1 227 Ac- 223 Recovery from Ra generators 227 The Ac method is characterized in that the inorganic acid adopted by the acid system is medical hydrochloric acid with the acid concentration not higher than 0.1 mol/L.
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| CN202311593599.XA CN117604283A (en) | 2023-11-24 | 2023-11-24 | A slave 227 Ac- 223 Recovery from Ra generators 227 Ac method |
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