CN116741428A - Based on accelerator irradiation 226 Ra simultaneous preparation 225 Ac and 212 pb method - Google Patents
Based on accelerator irradiation 226 Ra simultaneous preparation 225 Ac and 212 pb method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 97
- 229920005989 resin Polymers 0.000 claims abstract description 97
- 239000007788 liquid Substances 0.000 claims abstract description 75
- 239000002901 radioactive waste Substances 0.000 claims abstract description 34
- 238000000926 separation method Methods 0.000 claims abstract description 23
- 238000010894 electron beam technology Methods 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims description 210
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 92
- 150000007522 mineralic acids Chemical class 0.000 claims description 87
- 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 79
- 239000003729 cation exchange resin Substances 0.000 claims description 79
- 238000005406 washing Methods 0.000 claims description 49
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 42
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 36
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 34
- 229910017604 nitric acid Inorganic materials 0.000 claims description 34
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 28
- 238000001704 evaporation Methods 0.000 claims description 20
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- 230000001678 irradiating effect Effects 0.000 claims description 18
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- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000005262 alpha decay Effects 0.000 abstract description 5
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- 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
- G21G1/04—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes outside nuclear reactors or particle accelerators
- G21G1/12—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes outside nuclear reactors or particle accelerators by electromagnetic irradiation, e.g. with gamma or X-rays
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Abstract
The invention relates to an isotope preparation method, in particular to an accelerator-based irradiation method 226 Ra simultaneous preparation 225 Ac and 212 the Pb method aims at solving the defects of difficult acquisition of raw materials, difficult separation of impurities, complex operation and high requirement on separation equipment in the prior art. The invention converts high-power high-energy electron beam into bremsstrahlung bombardment 226 Ra sample target production 225 Ra and 224 Ra， 225 ra is produced by beta decay 225 Ac， 224 Ra is produced by alpha decay 212 Pb using 225 Ac and 212 differences in Pb growth rates and different resin pairs 225 Ac and 212 difference in Pb adsorption Performance 225 Ac and 212 pb was separated to obtain 225 Ac solution 212 Pb solution, improves the utilization rate of the device, reduces the production cost and reduces the radioactive waste liquid amount.
Description
Technical Field
The invention relates to an isotope preparation method, in particular to an accelerator-based irradiation method 226 Ra simultaneous preparation 225 Ac and 212 pb method.
Background
Along with the continuous updating and development of modern medicine on tumor diagnosis and treatment technology, tumor treatment is developing to accurate targeted treatment. In addition to targeted chemotherapeutic agents, targeted radionuclide therapeutic agents are becoming more and more important and have a very broad prospect. Radioisotopes attenuated by release of alpha particles, typically as 225 Ac and 212 pb is rapidly becoming an important field of tumor targeted therapy research, and preclinical animal experimental research and preliminary clinical practice have achieved very successful results. 225 Ac and 212 pb has great superiority for targeted therapy: 1) 225 Ac and 212 pb has excellent nuclear physical and chemical properties and short half life 225 Ac：9.9d； 212 Pb:10.6 h), and has small side effects. 2) 225 Ac and 212 pb and its daughter emit alpha particles with average energy of 6-8MeV, have very high Linear Energy Transfer (LET) in tissues, high deposition energy density of high LET radiation causes double strand break of a large amount of tumor cell DNA, has a large killing effect on the DNA in tumor cells, has a short action distance (about 2-100 microns, namely in the range of 6-8 cells), and has almost no toxic or side effect on normal tissues around tumor target tissues. 3) The radioisotope has good tissue biological effect, can be organically combined with polypeptide with short intake time, antibody for affinity blood cancer cells and the like, and forms strong tumor targeting.
Conventional ones 225 Ac is from 233 Extracted from decay chains of U 212 Pb was prepared from a large amount of 228 Separating and extracting the Th from the extract, 212 pb is uranium 232 U and 232 members of the Th decay chain, which can be defined by 228 Th(T 1/2 =1.9y) and 224 Ra(T 1/2 =3.66 d) decay and is divided by a cation exchange column 212 Removing other nuclides except Pb by chemical or physical separation, and washing with nitric acid or hydrochloric acid 212 Pb. Required by both 233 U and 228 th source starvation, nuclear material supervision problems, and complex decay chains are involved, the accumulated radioactive doses of various intermediates are very large, and the effect is realThe operation difficulty is high, the material performance requirement of the separation equipment is high, and more importantly 225 Ac and 212 pb yields are low and far from meeting the needs of research and clinic.
Disclosure of Invention
The invention aims to solve the defects of difficult acquisition of raw materials, difficult separation of impurities, complex operation and high requirement on separation equipment in the prior art, and provides the irradiation based on the accelerator 226 Ra simultaneous preparation 225 Ac and 212 pb method.
In order to achieve the above purpose, the technical solution provided by the present invention is as follows:
irradiation based on accelerator 226 Ra simultaneous preparation 225 Ac and 212 the Pb method is characterized by comprising the following steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator;
step 2, irradiating with X-rays 226 Ra sample targets, produced by nuclear reactions, respectively 225 Ra and 224 Ra；
step 3, irradiating 226 Dissolving the Ra sample target in an inorganic acid solution;
step 4, evaporating the inorganic acid solution obtained in the step 3, dissolving residues with the inorganic acid solution to obtain a solution A, standing for 1-3d, and transferring the solution A into a resin chromatographic column; the resin chromatographic column is an Sr resin chromatographic column or a Pb resin chromatographic column;
step 5, washing the resin chromatographic column with an inorganic acid solution, and collecting effluent; the inorganic acid is the same as the inorganic acid in the step 4;
step 6, separation and purification 212 Pb
Washing the resin chromatographic column again with inorganic acid solution, wherein the effluent liquid is first radioactive waste liquid; connecting the lower end of the resin chromatographic column with a first cation exchange resin chromatographic column, washing the resin chromatographic column and the first cation exchange resin column with a mixed solution of citric acid and sodium chloride, and collecting the effluent to obtain 212 A Pb solution;
step 7, separation and purification 225 Ac
Standing the effluent liquid in the step 5 for 15-20d, evaporating to dryness, dissolving residues with an inorganic acid solution, transferring the residues into a second cation exchange resin chromatographic column, then washing the second cation exchange resin chromatographic column with a perchloric acid solution, and collecting the effluent liquid as a second radioactive waste liquid; washing the second cation exchange resin chromatographic column with inorganic acid solution, and collecting effluent 225 Ac solution.
Further, the concentration of the mineral acid solution in the step 3 is 9+/-1 mol/L;
the concentration of the inorganic acid solution in the step 4 and the step 5 is 3+/-1 mol/L;
the volume of the inorganic acid solution in the step 5 is 2-4 times of the volume of the resin chromatographic column;
in the step 6, the concentration of the inorganic acid solution of the resin chromatographic column is 0.1+/-0.01 mol/L, and the volume of the inorganic acid solution is 10-20 times of that of the resin chromatographic column;
the concentrations of the citric acid and the sodium chloride in the mixed solution are 0.05+/-0.01 mol/L and 0.5+/-0.05 mol/L respectively; the pH=4.0+/-0.5 of the mixed solution, and the volume is 10-20 times of the volume of the resin chromatographic column;
in the step 7, the concentration of the inorganic acid solution for dissolving residues is 0.1+/-0.01 mol/L;
the concentration of the perchloric acid is 9+/-1 mol/L, and the volume of the perchloric acid is 2-4 times of that of the second cation exchange resin chromatographic column;
the concentration of the inorganic acid solution for washing the second cation exchange resin chromatographic column is 5+/-1 mol/L, and the volume of the inorganic acid solution is 2-4 times of that of the second cation exchange resin chromatographic column.
Further, in step 3 to step 7, the inorganic acid solution is a hydrochloric acid solution or a nitric acid solution.
Further, in step 1, the electron beam energy is greater than 25MeV; the irradiation time is 5-10d;
in the step 3, the inorganic acid solution is hydrochloric acid solution;
in the step 4 and the step 5, the inorganic acid solution is nitric acid solution;
in the step 6, the inorganic acid of the resin chromatographic column is washed again to be hydrochloric acid solution; the first cation exchange resin chromatographic column is a 50W multiplied by 8 chromatographic column;
in the step 7, the inorganic acid of the dissolved residues is hydrochloric acid solution, and the inorganic acid of the washing second cation exchange resin chromatographic column is nitric acid solution; the second cation exchange resin chromatographic column is a Dowex-50 chromatographic column.
At the same time, also provides a radiation based on accelerator 226 Ra simultaneous preparation 225 Ac and 212 the Pb method is characterized by comprising the following steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator;
step 2, irradiating with X-rays 226 Ra sample targets, produced by nuclear reactions, respectively 225 Ra and 224 Ra；
step 3, irradiating 226 Dissolving the Ra sample target in an inorganic acid solution;
step 4, evaporating the inorganic acid solution obtained in the step 3, dissolving residues with the inorganic acid solution to obtain a solution A, standing for 1-3d, and transferring the solution A into a resin chromatographic column; the resin chromatographic column is a Pb resin chromatographic column or an Sr resin chromatographic column;
step 5, washing the resin chromatographic column with an inorganic acid solution, and collecting effluent;
step 6, separation and purification 212 Pb
Washing the resin chromatographic column again with inorganic acid solution, wherein the effluent liquid is first radioactive waste liquid; connecting the lower end of the resin chromatographic column with a first cation exchange resin chromatographic column, washing the resin chromatographic column and the first cation exchange resin column with a mixed solution of citric acid and sodium chloride, and collecting the effluent to obtain 212 A Pb solution;
step 7, standing the effluent liquid in the step 5 for 2-4d, and adding the effluent liquid into a resin chromatographic column;
step 8, repeating the step 5, the step 6 and the step 7 for at least 4 times, so that the total standing time of the effluent liquid in the step 5 is 15-20d, and evaporating the effluent liquid obtained in the last step 5 to dryness to obtain corresponding residues;
step 9, separation and purification 225 Ac
Dissolving the residue with inorganic acid solution, transferring to a second cation exchange resin chromatographic column, washing the second cation exchange resin chromatographic column with perchloric acid solution, and collecting the effluent liquid as second radioactive waste liquid; washing the second cation exchange resin chromatographic column with inorganic acid solution, and collecting effluent 225 Ac solution.
Further, the method also comprises a step 10 of circularly treating the second radioactive waste liquid for 3-5 times:
standing the second radioactive waste liquid in the step 9 for 15-20 days, evaporating to obtain residue, circularly performing the step 9 on the obtained residue, and separating to obtain 225 Ac solution and corresponding second radioactive waste; circulating for 3-5 times, collecting each obtained 225 Ac solution and the resulting second radioactive waste.
Further, the concentration of the mineral acid solution in the step 3 is 9+/-1 mol/L;
the concentration of the inorganic acid solution in the step 4 and the step 5 is 3+/-1 mol/L;
the volume of the inorganic acid solution in the step 5 is 2-4 times of the volume of the resin chromatographic column;
in the step 6, the concentration of the inorganic acid solution of the resin chromatographic column is 0.1+/-0.01 mol/L, and the volume of the inorganic acid solution is 10-20 times of that of the resin chromatographic column;
the concentrations of the citric acid and the sodium chloride in the mixed solution are 0.05+/-0.01 mol/L and 0.5+/-0.05 mol/L respectively; the pH=4.0+/-0.5 of the mixed solution, and the volume is 10-20 times of the volume of the resin chromatographic column;
in the step 9, the concentration of the inorganic acid solution for dissolving residues is 0.1+/-0.01 mol/L;
the concentration of the perchloric acid is 9+/-1 mol/L, and the volume of the perchloric acid is 2-4 times of that of the second cation exchange resin chromatographic column;
the concentration of the inorganic acid solution for washing the second cation exchange resin chromatographic column is 5+/-1 mol/L, and the volume of the inorganic acid solution is 2-4 times of that of the second cation exchange resin chromatographic column.
Further, in the steps 3, 4, 5, 6 and 9, the inorganic acid solution is a hydrochloric acid solution or a nitric acid solution.
Further, in the step 1, electron beam energy of 25MeV is less than or equal to 70MeV; the irradiation time is 5-10d;
in the step 3, the inorganic acid solution is hydrochloric acid solution;
in the step 4 and the step 5, the inorganic acid solution is nitric acid solution;
in the step 6, the inorganic acid of the resin chromatographic column is washed again to be hydrochloric acid solution; the first cation exchange resin chromatographic column is a 50W multiplied by 8 chromatographic column;
in the step 9, the inorganic acid of the dissolved residues is hydrochloric acid solution, and the inorganic acid of the washing second cation exchange resin chromatographic column is nitric acid solution; the second cation exchange resin chromatographic column is a Dowex-50 chromatographic column.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the raw materials as 226 Ra, the production raw materials are easy to obtain, and the generated radioactive waste liquid is less; by bombardment of 226 Simultaneous production of Ra sample targets 225 Ac and 212 pb, reuse of different resin pairs 225 Ac and 212 the Pb was separated by the difference in adsorption property so that 226 The Ra sample target can be separated to obtain two medical isotopes after one irradiation, so that the utilization rate of the device is improved, and the production cost is reduced.
2. In the step 6.2 of the invention, every 2-4d returns to the step 5 in the standing process of effluent liquid, the treatment is repeated, and the effluent liquid is fully utilized 224 Ra (b); then the second radioactive waste liquid is circularly treated to lead the radioactive waste liquid to be 225 Ra is fully utilized, and the finally obtained second radioactive waste mainly contains 226 Ra, can be used for recovery of 226 Ra is recycled and effectively improves 212 Pb solution 225 The yield of Ac solution is reduced.
Drawings
FIG. 1 is a preparation flow chart of an embodiment of the present invention;
FIG. 2 is a schematic illustration of a first embodiment of the present invention 225 Ac α spectra;
FIG. 3 is a schematic illustration of a first embodiment of the invention 226 Ra after irradiation 225 Ra、 224 Attenuation of Ra 212 Pb、 209 Generating a relation diagram of Pb;
FIG. 4 shows a repeated separation in accordance with an embodiment of the present invention 225 Time profile of Ac.
Detailed Description
Example 1
The invention is based on accelerator irradiation 226 Ra simultaneous preparation 225 Ac and 212 pb method using high power high energy electron beam to convert it into bremsstrahlung bombardment 226 Ra sample target can be produced simultaneously 225 Ac and 212 pb, the method utilizes 225 Ac and 212 differences in Pb growth rates and different resin pairs 225 Ac and 212 pb adsorption performance difference, pb specific resin is firstly used for extracting from target dissolving solution 212 Pb, extracting with cation exchange resin 225 Ac, the purpose of obtaining two medical isotopes at the same time by one irradiation is achieved, so that the utilization rate of the device is improved, and the production cost is reduced. Wherein,, 212 pb and 225 the reaction of Ac formation is as follows:
the preparation flow chart of the method is shown in fig. 1, and comprises the following steps:
step 1, generating X-rays by utilizing an electron beam with the energy of an electron accelerator of 40 MeV;
wherein, the electron beam energy is less than or equal to 25MeV and less than or equal to 70MeV, and preferably 40MeV.
Step 2, irradiating with X-rays 226 The Ra sample was targeted for 9 days, 226 ra sample target through Nuclear reaction 226 Ra (gamma, n) generation 225 Ra, and, at the same time, 226 ra sample target through Nuclear reaction 226 Ra (gamma, 2 n) generation 224 Ra；
The irradiation time is usually 5-10d, rootDepending on the amount of product desired; during irradiation, a small amount of decay reactions occur: 225 ra decays beta to 225 Ac， 224 Ra is produced by 3 times of alpha decay 212 Pb；
Step 3, irradiating 226 Dissolving the Ra sample target in hydrochloric acid solution; the concentration of the hydrochloric acid solution is 9+/-1 mol/L, and the volume of the hydrochloric acid solution is determined according to the mass of the sample target, so that the sample target is completely dissolved;
step 4, evaporating the hydrochloric acid solution to dryness, and dissolving residues with 3mL of nitric acid solution to obtain a solution A; standing the solution A for 3d, and transferring the solution A into a Sr resin chromatographic column;
the concentration of the nitric acid solution is 3+/-1 mol/L, the volume of the nitric acid solution is 2-5mL, and the volume of the nitric acid solution is adjusted according to the amount of the residue, so that the residue can be completely dissolved; the rest time is usually 2-4 days, so that 224 Ra is produced by 3 times of alpha decay 212 Pb, too long or too short a time, may cause 212 Reduction of Pb product content, as shown in FIG. 3 226 After the Ra is irradiated, the light is irradiated, 225 Ra、 224 attenuation of Ra 212 Pb、 209 Generating a relation diagram of Pb.
Step 5, washing the Sr resin chromatographic column with 2mL of nitric acid solution, and collecting effluent liquid; the concentration of nitric acid solution for washing the Sr resin chromatographic column is 3+/-1 mol/L.
The nitric acid solution has good effect when the volume of the nitric acid solution is about 2-4 times of the volume of the Sr resin chromatographic column, and the volume of the nitric acid solution is usually 2-4mL according to the volume of the Sr resin chromatographic column.
Step 6, separation and purification
6.1. Separation and purification 212 Pb
Washing the Sr resin chromatographic column again by using 10mL of hydrochloric acid solution, wherein the effluent liquid is first radioactive waste liquid; the concentration of the hydrochloric acid solution is 0.1+/-0.01 mol/L.
Then the lower end of the Sr resin chromatographic column is connected with a first cation exchange resin chromatographic column, the Sr resin chromatographic column and the first cation exchange resin chromatographic column are washed by 10mL of mixed solution of citric acid and sodium chloride, and the effluent liquid is collected 212 A Pb solution;
in the present invention, the volume of the hydrochloric acid solution is about 10 to 20 times the volume of the Sr resin chromatographic column and about 10 to 20mL. The concentration of citric acid in the mixed solution is 0.05+/-0.01 mol/L, the concentration of sodium chloride is 0.5+/-0.05 mol/L, the pH value of the mixed solution is=4.0+/-0.5, the volume is 10-20mL, and the volume is about 10-20 times of the volume of the Sr resin chromatographic column.
Wherein the first cation exchange resin chromatographic column is a 50W multiplied by 8 chromatographic column or other cation exchange columns with similar effects.
6.2. Separation and purification 225 Ac
Standing the effluent liquid in the step 5 for 16d, evaporating to dryness, dissolving residues by using hydrochloric acid solution, transferring the residues into a second cation exchange resin chromatographic column, then washing the second cation exchange resin chromatographic column by using 10mL of perchloric acid for removing Al, fe, mg, ra, pa, po, pb and Bi, and collecting the effluent liquid as second radioactive waste liquid; washing the second cation exchange resin chromatographic column with 10mL nitric acid solution, and collecting effluent to obtain 225 Ac solution.
The second cation exchange resin chromatographic column is a Dowex-50 chromatographic column or other cation exchange columns with similar effects. The concentration of the hydrochloric acid solution for dissolving the residues is 0.1+/-0.01 mol/L, and the volume is 2-5mL, so that the residues are completely dissolved; the concentration of the perchloric acid is 9+/-1 mol/L, the volume is 5-10mL, and the concentration is about 2-4 times of the volume of the second cation exchange resin chromatographic column; the concentration of nitric acid solution for washing the second cation exchange resin chromatographic column is 5+/-1 mol/L, the volume is 5-10mL, and the volume is about 2-4 times of the volume of the second cation exchange resin chromatographic column.
The standing time can be 15-20d, so that 225 Ra decays beta to 225 Ac, too long a time, can result in 225 The Ac product content is reduced, the time is too short, and a small amount of Ac product is also contained in effluent liquid 224 Ra and products thereof 212 Pb, etc., generates interference, 15-20d is about 224 Ra half-life was 5 times 3.66d, when the vast majority 224 Ra has decayed.
In the invention, the granularity of Sr resin in Sr resin chromatographic column is 50-100 mu m, the effective volume of the column is 500-1000 mu L, and the column is filled by adopting a sedimentation method; the granularity of cation exchange resin in the first cation exchange resin chromatographic column is 100-150 mu m, the effective volume of the column is 500-1000 mu L, and the column is filled by adopting a sedimentation method; the size of cation exchange resin in the second cation exchange resin chromatographic column is 200 meshes, the effective volume of the column is 500-2000 mu L, and the column is filled by adopting a sedimentation method. The smaller the particle size of Sr resin and the mesh number of cation exchange resin, the better the resin adsorption performance of the same quality, but the smaller the resin has too great resistance to passing liquid, influences the flow rate of the liquid and increases the separation time, so that the proper particle size and mesh number are required to be selected to have better effect.
In other embodiments of the present invention, the hydrochloric acid solution, nitric acid solution may be replaced with other inorganic acid solutions, and the Sr resin chromatography column may be replaced with a Pb resin chromatography column.
With a resolution of 16keV and an active area of 0.6cm 2 Alpha Si (Au) detector pair end product 225 The Ac solution was subjected to alpha ray measurement. Coating the stainless steel carrier with 225 Ac solution, then evaporated 225 Ac solution is prepared into an alpha sample, and the alpha spectrum of the alpha sample is obtained by measuring the alpha sample, as shown in figure 2, it can be seen that 225 The four alpha decay nuclides in the Ac decay chain are clear, and the energy is Ealpha #, respectively 225 Ac)＝5.8MeV，Eα( 221 Fr)＝6.3MeV，Eα( 217 At)＝7.1MeV，Eα( 213 Po) =8.4 MeV, and at the same time, other alpha decay nuclides are not visible in the figure, indicating that the invention obtained 225 The Ac purity is very high, and meets the requirement.
The effluent of step 5 contains 226 Ra、 225 Ra and 224 ra, standing for 15-20d in step 6.2 to remove 224 Ra (b); wherein when the mixture is kept stand for 2 to 4 days, 224 ra decay production 212 Pb, thus, in the process of standing for 15-20d, transferring it to Sr resin chromatographic column every 2-4d, returning to step 5 for treatment, collecting the produced 212 Pb, thereby improving 212 And (3) the yield of Pb solution, and repeating for at least 4 times until the total standing time of the effluent reaches 15-20d, and then entering the step 6.2. At this time, the second radioactive waste liquid obtained in the step 6.2 contains 226 Ra and 225 ra (b); FIG. 4 shows the effluent of step 5 when it is stationary, wherein 225 Ac and 225 isolation time map of RaAccording to the change, every 15-20 days, 225 the activity of Ac will tend to stabilize, and after more than 20 days, 225 since Ac activity tends to decrease instead, according to FIG. 4, the effluent is left to stand for about 15 to 20 days in step 6.2 and then separated, and the effluent in step 5 is replaced with the obtained second radioactive waste liquid, and the process is circulated for 3 to 5 times in step 6.2, thereby obtaining the second radioactive waste liquid 225 The Ra activity is reduced to the minimum, and the main component is 226 Ra, can be used for 226 Recycling Ra while collecting each cycle generation 225 Ac solution, effectively improve 225 Yield of Ac solution.
Example two
The invention is based on accelerator irradiation 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb comprising the steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator; the electron beam energy was 35MeV;
step 2, irradiating with X-rays 226 The Ra sample target was taken for 5 days, 226 ra sample target through Nuclear reaction 226 Ra (gamma, n) generation 225 Ra， 226 Ra sample target through Nuclear reaction 226 Ra (gamma, 2 n) generation 224 Ra；
Step 3, irradiating 226 Dissolving the Ra sample target in hydrochloric acid solution;
step 4, evaporating the hydrochloric acid solution to dryness, and dissolving residues with 2mL of hydrochloric acid solution to obtain a solution A;
step 5, standing the solution A for 3d, transferring the solution A into an Sr resin chromatographic column, washing the Sr resin chromatographic column with 3mL of hydrochloric acid solution, and collecting effluent liquid;
step 6, separation and purification
6.1. Washing the Sr resin chromatographic column again by using 14mL of hydrochloric acid solution, wherein the effluent liquid is first radioactive waste liquid;
then the lower end of the Sr resin chromatographic column is connected with a first cation exchange resin chromatographic column, the Sr resin chromatographic column and the first cation exchange resin chromatographic column are washed by 14mL of mixed solution of citric acid and sodium chloride, and the effluent liquid is collected 212 A Pb solution;
6.2. standing the effluent liquid in the step 5 for 15d, evaporating to dryness, dissolving residues by using hydrochloric acid solution, transferring the residues into a second cation exchange resin chromatographic column, then washing the second cation exchange resin chromatographic column by using 7mL of perchloric acid for removing Al, fe, mg, ra, pa, po, pb and Bi, and collecting the effluent liquid as second radioactive waste liquid; washing the second cation exchange resin chromatographic column with 7mL nitric acid solution, and collecting effluent to obtain 225 Ac solution.
Example III
The invention is based on accelerator irradiation 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb comprising the steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator; the electron beam energy was 70MeV;
step 2, irradiating with X-rays 226 The Ra sample was targeted for 8 days, 226 ra sample target through Nuclear reaction 226 Ra (gamma, n) generation 225 Ra， 226 Ra sample target through Nuclear reaction 226 Ra (gamma, 2 n) generation 224 Ra；
Step 3, irradiating 226 Dissolving the Ra sample target in hydrochloric acid solution;
step 4, evaporating the hydrochloric acid solution to dryness, and dissolving residues with 5mL of nitric acid solution to obtain a solution A;
step 5, after standing the solution A for 2d, transferring the solution A into an Sr resin chromatographic column, washing the Sr resin chromatographic column by using 4mL of nitric acid solution, and collecting effluent liquid;
step 6, separation and purification
6.1. Washing the Sr resin chromatographic column again by using 20mL of nitric acid solution, wherein the effluent liquid is first radioactive waste liquid;
then the lower end of the Sr resin chromatographic column is connected with a first cation exchange resin chromatographic column, the Sr resin chromatographic column and the first cation exchange resin chromatographic column are washed by 20mL of mixed solution of citric acid and sodium chloride, and the effluent liquid is collected 212 A Pb solution;
6.2. standing the effluent in step 5 for 20d, evaporating to dryness, dissolving the residue with hydrochloric acid solution, and transferring to the first stepWashing the second cation exchange resin chromatographic column with 8mL perchloric acid for removing Al, fe, mg, ra, pa, po, pb and Bi, and collecting the effluent liquid as second radioactive waste liquid; washing the second cation exchange resin chromatographic column with 8mL hydrochloric acid solution, and collecting the effluent to obtain 225 Ac solution.
Example IV
The invention is based on accelerator irradiation 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb comprising the steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator; the electron beam energy was 25MeV;
step 2, irradiating with X-rays 226 The Ra sample target was taken for 10 days, 226 ra sample target through Nuclear reaction 226 Ra (gamma, n) generation 225 Ra, and, at the same time, 226 ra sample target through Nuclear reaction 226 Ra (gamma, 2 n) generation 224 Ra；
Step 3, irradiating 226 Dissolving the Ra sample target in hydrochloric acid solution;
step 4, evaporating the hydrochloric acid solution to dryness, and dissolving residues with 5mL of nitric acid solution to obtain a solution A;
step 5, standing the solution A for 3d, transferring the solution A into an Sr resin chromatographic column, washing the Sr resin chromatographic column by using 3.5mL of nitric acid solution, and collecting effluent liquid;
step 6, separation and purification
6.1. Washing the Sr resin chromatographic column again by 16mL of hydrochloric acid solution, wherein the effluent liquid is first radioactive waste liquid;
then the lower end of the Sr resin chromatographic column is connected with a first cation exchange resin chromatographic column, the Sr resin chromatographic column and the first cation exchange resin chromatographic column are washed by 16mL of mixed solution of citric acid and sodium chloride, and the effluent liquid is collected 212 A Pb solution;
6.2. standing the effluent from step 5 for 18d, evaporating to dryness, dissolving the residue with hydrochloric acid solution, transferring to a second cation exchange resin column, and washing the second cation exchange resin column with 9mL perchloric acid for removing Al, fe, mg, ra, pa,Po, pb and Bi, and collecting effluent liquid as second radioactive waste liquid; washing the second cation exchange resin chromatographic column with 9mL hydrochloric acid solution, and collecting the effluent to obtain 225 Ac solution.
Example five
The invention is based on accelerator irradiation 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb comprising the steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator; the electron beam energy was 55MeV;
step 2, irradiating with X-rays 226 The Ra sample target was taken for 7 days, 226 ra sample target through Nuclear reaction 226 Ra (gamma, n) generation 225 Ra, and, at the same time, 226 ra sample target through Nuclear reaction 226 Ra (gamma, 2 n) generation 224 Ra；
Step 3, irradiating 226 Dissolving the Ra sample target in hydrochloric acid solution;
step 4, evaporating the hydrochloric acid solution to dryness, and dissolving residues with 4mL of nitric acid solution to obtain a solution A;
step 5, after standing the solution A for 1d, transferring the solution A into an Sr resin chromatographic column, washing the Sr resin chromatographic column by using 3mL of nitric acid solution, and collecting effluent liquid;
step 6, separation and purification
6.1. Washing the Sr resin chromatographic column again by 13mL of hydrochloric acid solution, wherein the effluent liquid is first radioactive waste liquid;
then the lower end of the Sr resin chromatographic column is connected with a first cation exchange resin chromatographic column, the Sr resin chromatographic column and the first cation exchange resin chromatographic column are washed by 12mL of mixed solution of citric acid and sodium chloride, and the effluent liquid is collected 212 A Pb solution;
6.2. standing the effluent liquid in the step 5 for 16d, evaporating to dryness, dissolving residues by using hydrochloric acid solution, transferring the residues into a second cation exchange resin chromatographic column, then washing the second cation exchange resin chromatographic column by using 5mL of perchloric acid for removing Al, fe, mg, ra, pa, po, pb and Bi, and collecting the effluent liquid as second radioactive waste liquid; washing the second cation exchange resin chromatographic column with 5mL nitric acid solution, and collecting effluent to obtain 225 Ac solution.
Claims (9)
1. Irradiation based on accelerator 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb, comprising the steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator;
step 2, irradiating with X-rays 226 Ra sample targets, produced by nuclear reactions, respectively 225 Ra and 224 Ra；
step 3, irradiating 226 Dissolving the Ra sample target in an inorganic acid solution;
step 4, evaporating the inorganic acid solution obtained in the step 3, dissolving residues with the inorganic acid solution to obtain a solution A, standing for 1-3d, and transferring the solution A into a resin chromatographic column; the resin chromatographic column is an Sr resin chromatographic column or a Pb resin chromatographic column;
step 5, washing the resin chromatographic column with an inorganic acid solution, and collecting effluent; the inorganic acid used for washing the resin chromatographic column is the same as the inorganic acid in the step 4;
step 6, separation and purification 212 Pb
Washing the resin chromatographic column again with inorganic acid solution, wherein the effluent liquid is first radioactive waste liquid; connecting the lower end of the resin chromatographic column with a first cation exchange resin chromatographic column, washing the resin chromatographic column and the first cation exchange resin column with a mixed solution of citric acid and sodium chloride, and collecting the effluent to obtain 212 A Pb solution;
step 7, separation and purification 225 Ac
Standing the effluent liquid in the step 5 for 15-20d, evaporating to dryness, dissolving residues with an inorganic acid solution, transferring the residues into a second cation exchange resin chromatographic column, then washing the second cation exchange resin chromatographic column with a perchloric acid solution, and collecting the effluent liquid as a second radioactive waste liquid; washing the second cation exchange resin chromatographic column with inorganic acid solution, and collecting effluent 225 Ac solution.
2. The accelerator-based irradiation of claim 1 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb characterized by:
the concentration of the inorganic acid solution in the step 3 is 9+/-1 mol/L;
the concentration of the inorganic acid solution in the step 4 and the step 5 is 3+/-1 mol/L;
the volume of the inorganic acid solution in the step 5 is 2-4 times of the volume of the resin chromatographic column;
in the step 6, the concentration of the inorganic acid solution of the resin chromatographic column is 0.1+/-0.01 mol/L, and the volume of the inorganic acid solution is 10-20 times of that of the resin chromatographic column;
the concentrations of the citric acid and the sodium chloride in the mixed solution are 0.05+/-0.01 mol/L and 0.5+/-0.05 mol/L respectively; the pH=4.0+/-0.5 of the mixed solution, and the volume is 10-20 times of the volume of the resin chromatographic column;
in the step 7, the concentration of the inorganic acid solution for dissolving residues is 0.1+/-0.01 mol/L;
the concentration of the perchloric acid is 9+/-1 mol/L, and the volume of the perchloric acid is 2-4 times of that of the second cation exchange resin chromatographic column;
the concentration of the inorganic acid solution for washing the second cation exchange resin chromatographic column is 5+/-1 mol/L, and the volume of the inorganic acid solution is 2-4 times of that of the second cation exchange resin chromatographic column.
3. Accelerator-based irradiation according to claim 1 or 2 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb characterized by:
in the steps 3 to 7, the inorganic acid solution is hydrochloric acid solution or nitric acid solution.
4. The accelerator-based irradiation of claim 3 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb characterized by:
in step 1, the electron beam energy is greater than 25MeV; the irradiation time is 5-10d;
in the step 3, the inorganic acid solution is hydrochloric acid solution;
in the step 4 and the step 5, the inorganic acid solution is nitric acid solution;
in the step 6, the inorganic acid of the resin chromatographic column is washed again to be hydrochloric acid solution; the first cation exchange resin chromatographic column is a 50W multiplied by 8 chromatographic column;
in the step 7, the inorganic acid of the dissolved residues is hydrochloric acid solution, and the inorganic acid of the washing second cation exchange resin chromatographic column is nitric acid solution; the second cation exchange resin chromatographic column is a Dowex-50 chromatographic column.
5. Irradiation based on accelerator 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb, comprising the steps of:
step 1, generating X rays by utilizing an electron beam of an electron accelerator;
step 2, irradiating with X-rays 226 Ra sample targets, produced by nuclear reactions, respectively 225 Ra and 224 Ra；
step 3, irradiating 226 Dissolving the Ra sample target in an inorganic acid solution;
step 4, evaporating the inorganic acid solution obtained in the step 3, dissolving residues with the inorganic acid solution to obtain a solution A, standing for 1-3d, and transferring the solution A into a resin chromatographic column; the resin chromatographic column is a Pb resin chromatographic column or an Sr resin chromatographic column;
step 5, washing the resin chromatographic column with an inorganic acid solution, and collecting effluent;
step 6, separation and purification 212 Pb
Washing the resin chromatographic column again with inorganic acid solution, wherein the effluent liquid is first radioactive waste liquid; connecting the lower end of the resin chromatographic column with a first cation exchange resin chromatographic column, washing the resin chromatographic column and the first cation exchange resin column with a mixed solution of citric acid and sodium chloride, and collecting the effluent to obtain 212 A Pb solution;
step 7, standing the effluent liquid in the step 5 for 2-4d, and adding the effluent liquid into a resin chromatographic column;
step 8, repeating the step 5, the step 6 and the step 7 for at least 4 times, so that the total standing time of the effluent liquid in the step 5 is 15-20d, and evaporating the effluent liquid obtained in the last step 5 to dryness to obtain corresponding residues;
step 9, separation and purification 225 Ac
Dissolving the residue with inorganic acid solution, transferring to a second cation exchange resin chromatographic column, washing the second cation exchange resin chromatographic column with perchloric acid solution, and collecting the effluent liquid as second radioactive waste liquid; washing the second cation exchange resin chromatographic column with inorganic acid solution, and collecting effluent 225 Ac solution.
6. The accelerator-based irradiation of claim 5 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb characterized by: and the method also comprises a step 10 of circularly treating the second radioactive waste liquid for 3-5 times:
standing the second radioactive waste liquid in the step 9 for 15-20 days, evaporating to obtain residue, circularly performing the step 9 on the obtained residue, and separating to obtain 225 Ac solution and corresponding second radioactive waste; circulating for 3-5 times, collecting each obtained 225 Ac solution and the resulting second radioactive waste.
7. The accelerator-based irradiation of claim 6 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb characterized by:
the concentration of the inorganic acid solution in the step 3 is 9+/-1 mol/L;
the concentration of the inorganic acid solution in the step 4 and the step 5 is 3+/-1 mol/L;
the volume of the inorganic acid solution in the step 5 is 2-4 times of the volume of the resin chromatographic column;
in the step 6, the concentration of the inorganic acid solution of the resin chromatographic column is 0.1+/-0.01 mol/L, and the volume of the inorganic acid solution is 10-20 times of that of the resin chromatographic column;
the concentrations of the citric acid and the sodium chloride in the mixed solution are 0.05+/-0.01 mol/L and 0.5+/-0.05 mol/L respectively; the pH=4.0+/-0.5 of the mixed solution, and the volume is 10-20 times of the volume of the resin chromatographic column;
in the step 9, the concentration of the inorganic acid solution for dissolving residues is 0.1+/-0.01 mol/L;
the concentration of the perchloric acid is 9+/-1 mol/L, and the volume of the perchloric acid is 2-4 times of that of the second cation exchange resin chromatographic column;
the concentration of the inorganic acid solution for washing the second cation exchange resin chromatographic column is 5+/-1 mol/L, and the volume of the inorganic acid solution is 2-4 times of that of the second cation exchange resin chromatographic column.
8. The accelerator-based irradiation of claim 7 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb characterized by:
in the steps 3, 4, 5, 6 and 9, the inorganic acid solution is hydrochloric acid solution or nitric acid solution.
9. The accelerator-based irradiation of claim 8 226 Ra simultaneous preparation 225 Ac and 212 a method of Pb characterized by:
in the step 1, the electron beam energy is less than or equal to 25MeV and less than or equal to 70MeV; the irradiation time is 5-10d;
in the step 3, the inorganic acid solution is hydrochloric acid solution;
in the step 4 and the step 5, the inorganic acid solution is nitric acid solution;
in the step 6, the inorganic acid of the resin chromatographic column is washed again to be hydrochloric acid solution; the first cation exchange resin chromatographic column is a 50W multiplied by 8 chromatographic column;
in the step 9, the inorganic acid of the dissolved residues is hydrochloric acid solution, and the inorganic acid of the washing second cation exchange resin chromatographic column is nitric acid solution; the second cation exchange resin chromatographic column is a Dowex-50 chromatographic column.
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