CN101468791B - Extraction and purification technique for producing iodine-131 using homogeneous solution-type reactor - Google Patents

Extraction and purification technique for producing iodine-131 using homogeneous solution-type reactor Download PDF

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CN101468791B
CN101468791B CN2007103060555A CN200710306055A CN101468791B CN 101468791 B CN101468791 B CN 101468791B CN 2007103060555 A CN2007103060555 A CN 2007103060555A CN 200710306055 A CN200710306055 A CN 200710306055A CN 101468791 B CN101468791 B CN 101468791B
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李茂良
程作用
邓启民
柴德安
李海颖
冯义红
李明起
张劲松
陈云明
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Nuclear Power Institute of China
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Abstract

The invention belongs to the technology of producing medical radioactive nuclide, and in particular relates to a process for extracting and purifying iodine-131 through a homogeneous aqueous solution nuclear reactor. The process comprises the following steps: adsorbing iodine-131 is from a bulk fuel solution after the reactor operates by an aluminum oxide extraction column or a hydrous zirconium oxide extraction column; and then cleaning the extraction column by using diluted HNO3, H2O, NH3.H2O; desorbing the iodine-131 on the extraction column by an NH3.H2O or NaOH solution; and finally, separating and purifying the desorbed iodine-131. The yield of the <131>I obtained by the process is more than 50 percent, and purity of the <131>I meets the requirement of a medical Na<131>I solution.

Description

Produce the extraction and purification technology of iodine-131 with uniform water solution nuclear reactor
Technical field
The invention belongs to the production technology of medical radionuclide, be specifically related to a kind of extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor.
Background technology
Iodine-131 is important medical radionuclide, be nuclear medicine treatment usefulness the earliest, maximum isotropic substance, iodine-131 treatment hyperthyroidism and first cancer are universally acknowledged effect methods, the monoclonal antibody of the iodine-131 mark that develops gradually in recent years is used for tumor treatment in addition, further advanced the application of iodine-131 again, so market is to the also increase gradually of demand of iodine-131.
Usually iodine-131 utilizes neutron activation
Figure S2007103060555D00011
Or 235U fission target spare method ( 235U (n, f) 131I) produce, but small scale, it is many to produce radwaste, the production cost height.Utilization is with UO 2(NO 3) 2Solution is that the homogeneity nuclear reactor of nuclear fuel is produced iodine-131, can accomplish scale production, and, can generate with 200kW power operation 24 hours as this reactor 131The about 15TBg of I (400Ci).Utilize this method to produce 131It is few that I produces refuse, and cost is low, has dissemination.Produce medical in the past 131The I product all utilizes distillation method, and the fuel solution volume of uniform water solution nuclear reactor big (about 100L), distillation method can't realize.Therefore, need research and development a kind of be applicable to the radioiodine that from water solution nuclear reactor large volume fuel solution, extracts trace (several milligrams) ( 131I and 131I) technology, and carry out purifying, allow 133I decay to the permission level, makes it to be used for nuclear medicine diagnostic and treatment.
With UO 2(NO 3) 2Solution is that the U concentration of fuel solution of the uniform water solution nuclear reactor of nuclear fuel is about 50mg/mL, HNO 3Concentration is 0.1-0.3mol/L.Produce a large amount of fission products during reactor operation, the valence state more complicated of fission product iodine in acidic solution mainly contains I -, I 2, IO 3-Equivalent state.I -By H 2The O radiolysis produces H 2O 2Be oxidized to I 2, evaporable I from fuel solution 2In entering air circuit again can with water in the fuel solution or with air circuit in water reaction under the spray generate I -And IO -, IO -Oxidized again generation IO 3 -(or IO 4 -).Because the iodine in the fuel solution is mainly with IO 3 -Form exists, so extract from fuel solution 131I is primarily aimed at IO 3 -Carry out.For extract iodine from uniform water solution nuclear reactor fuel solution, it is crucial selecting suitable iodine exchanger.Require exchanger still can not adsorb uranium iodine absorption, also necessary anti-irradiation and stable performance can repeat repeatedly to use, and can not introduce new impurity to fuel solution.
Summary of the invention
The objective of the invention is at the bulky characteristics of uniform water solution nuclear reactor fuel solution, the extraction and purification technology with uniform water solution nuclear reactor production iodine-131 that a kind of purification effect is good, the rate of recovery is high is provided.
Technical scheme of the present invention is as follows: a kind of extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor, this technology is adsorbed iodine-131 with aluminium sesquioxide extraction column or hydrous zirconium oxide extraction column the large volume fuel solution after reactor operation, uses rare HNO then successively 3, H 2O, NH 3H 2O cleans extraction column, uses NH again 3H 2Iodine-131 on O or the NaOH solution stripping extraction column carries out separation and purification to the iodine-131 after the desorb at last.
Aforesaid extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor, wherein, the volume of aluminium sesquioxide extraction column or hydrous zirconium oxide extraction column is for extracting 1/100～1/50 of feed liquid, and the height of extraction column and diameter ratio are 2～6; Extraction column is before use through the presaturation of 0.1～0.3mol/L of 3.5～7 times of column volumes salpeter solution; The flow velocity of solution is 0.5～2.0ml/ml/min during absorption.
Aforesaid extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor, wherein, the scavenging solution that cleans extraction column is that the concentration of 3.5～7 times of column volumes is that the concentration of the water of 0.1～0.3mol/L nitric acid, 3.5～7 times of column volumes, 3.5～7 times of column volumes is the NH of 0.01mol/L 3H 2O; The flow velocity of three kinds of scavenging solutions is 0.5-2.0mL/mL/min.
Aforesaid extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor wherein, during iodine-131 on the desorb extraction column, is 1～2mol/L NH with the concentration of 2.5～7 times of column volumes 3H 2O, desorb flow velocity are 0.5～2.0mL/mL/min; Perhaps the concentration with 2.5～7 times of column volumes is 0.2～1.0mol/LNaOH solution, and the desorb flow velocity is 0.5～2.0mL/mL/min.
Aforesaid extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor wherein, is carried out separation and purification to the iodine-131 after the desorb and is comprised the steps:
(1) stripping liquid of extraction column being adjusted to concentration of nitric acid with concentrated nitric acid is 0.1～0.3mol/L acidic medium, again by volume aluminium sesquioxide or the hydrous zirconium oxide purification column little than extraction column; The volume of purification column is to be purified 1/50～1/20 of feed liquid, and the height of purification column is 2～6 with the diameter ratio, through 3.5～7 times of column volume 0.1～0.3mol/L HNO 3Adsorb after the solution presaturation, the flow velocity of absorption iodine-131 is 0.5～2.0mL/mL/min again;
(2) be the HNO of 0.1～0.3mol/L with the concentration of 3.5～7 times of column volumes successively to the purification column behind the absorption iodine-131 3Solution, the H of 3.5～7 times of column volumes 2O, the concentration of 2.5～7 times of column volumes is 0.01mol/L NH 3H 2O solution cleans, and the flow velocity of three kinds of scavenging solutions is 0.5-2.0mL/mL/min;
(3) be 1～2mol/L NH with 2.5～7 times of column volume concentration 3H 2O is from aluminium sesquioxide purification column desorb iodine-131, or with the concentration of 2.5～7 times of column volumes be 0.2～1.0mol/L NaOH from hydrous zirconium oxide purification column desorb iodine-131, the desorb flow velocity is 0.5-2.0mL/mL/min.
Aforesaid extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor, wherein, as Na from the purification column desorb 131I solution or NH 4 131Contain in the I solution 99MoO 4 -During negative ion impurity, the stripping liquid of regulating purification column with HCl is used Na again to acid 2SO 3Or Na 2S 2O 4Will 131IO 3 -Be reduced to 131I -, by second aluminium sesquioxide or hydrous zirconium oxide purification column, the concentration with 3.5～7 times of column volumes is 0.1～0.3mol/LHNO then again 3Solution, the H of 3.5～7 times of column volumes 2O, 3.5～7 times of column volume concentration are that 0.01mol/LNaOH solution cleans successively, the concentration with 2.5～7 times of column volumes is that 0.2～1.0mol/LNaOH solution stripping I-131 can get Na at last 131The I solution product, the desorb flow velocity is 0.5-2.0mL/mL/min.
Aforesaid extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor, wherein, when from the iodine-131 solution of purification column desorb, containing 99MoO 4 -During negative ion impurity,, get Na at last with conventional distillation method purifying I-131 131The I solution product.
Technology of the present invention is applicable to from UO 2(NO 3) 2Solution is to extract purifying I-131 in the fuel solution of uniform water solution nuclear reactor of nuclear fuel, can obtain medical I-131 product, also can be used to extract purifying Mo-99 simultaneously, obtains medical Mo-99 product.This technology obtains 131The yield of I is greater than 50%, and its purity satisfies medical Na 131The requirement of I solution.
Description of drawings
Fig. 1 is three Al 2O 3Post extracts purifying molybdenum and iodine schema simultaneously.
Fig. 2 is 125The adsorption process figure of I spike simulation post III.
Fig. 3 is that uniform water solution nuclear reactor bench simulation test Mo and I extract and the purifying schema.
Fig. 4 is for extracting purifying iodine-131 simulation test platform system schematic diagram.
Among Fig. 4,1. volume pump 2. extraction columns 3. feed liquid transferpumps 4. reactor fuel containers 5. purification columns 6. separator columns 7. leacheate collection containers 8. leacheate collection containers 9. 131I product collection container 10. 99Temporary jar of Mo product collection container 11. fuel solutions
Embodiment
Below in conjunction with laboratory study and bench simulation test the present invention is described in detail.
Liquid phase 131I extracts the selection research that exchanger is at first carried out in experiment, promptly studies nitric acid system
Figure DEST_PATH_GSB00000313707400021
In exchanger to the absorption property of iodine and select desorption condition, study then in the uranyl nitrate system (
Figure DEST_PATH_GSB00000313707400022
Cu=50mg/mL) exchanger is to the extraction performance of iodine, and the iodine in the experiment uses inactive NaI and NaIO 3, the concentration (C of iodine in the adsorption liquid in the experiment I=1ug/mL) roughly the same with the iodine amount of uniform water solution nuclear reactor generation in service, uranyl nitrate solution in the experiment uses the natural uranium preparation, the research of chamber selects suitable liquid phase iodine to extract the exchanger and the preliminary technology of determining extraction of usefulness by experiment, by 1: 1 platform experiment the extraction process of liquid phase iodine is verified at last.
Selected hydrous zirconium oxide (HZO) for use in laboratory study, acid alchlor (Al 2O 3), platinum charcoal (Pt-C) and gac etc. have carried out IO 3 -Absorption and desorption experiment.Extraction column adopts Φ 8mm glass column, and the height of extraction column and diameter ratio are 2-6, needs through 3.5-7 times of column volume 0.1-0.5mol/L HNO before extraction column uses 3The solution presaturation.The HNO of testing liquid 3Concentration is 0.1-0.5mol/L, with NaIO 3The iodine concentration that form exists is 1ug/mL, and the adsorbent solution volume is 50-100 a times of extraction column, and solution upper prop absorption flow velocity is 0.5-2.0mL/mL/min, is 0.1-0.3mol/L HNO with 3.5-7 times of column volume concentration respectively after absorption is finished 3, 3.5-7 times of column volume H 2O, 3.5-7 times of column volume concentration is 0.01mol/L NH 3H 2O cleans, and the flow velocity of three kinds of scavenging solutions is 0.5-2.0mL/mL/min.Having cleaned the back is 0.1-2.0mol/L NH with 2.5-7 times of column volume concentration 3H 2O, or 2.5-7 times of column volume concentration is the iodine on the 0.1-1.0mol/LNaOH solution stripping extraction column, and the desorb flow velocity is 0.5-2.0mL/mL/min.Experimental studies results shows that the extraction column volume is better for the 1/50-1/100 that extracts material liquid volume, and the height of extraction column and the ratio 3-5 of diameter are best, the HNO of testing liquid 3Concentration is that 0.1-0.3mol/L is best, Al 2O 3Extraction column 1-2mol/L NH 3H 2The O desorb is best, and the HZO extraction column is best with 0.2-1.0mol/L NaOH solution stripping.Utilize Φ 8mm extraction column, extraction agent is 1.2mL, and 100mL is contained NaIO 3Solution (iodine concentration is 1ug/mL) adsorbs and desorption experiment, the results are shown in Table 1.
The different exchangers of table 1 are to ionic adsorption and desorb test-results
Figure 2007103060555A00800051
Table 1 data show that Pt-C and gac can not be used for extracting with IO 3 -The iodine that ionic species exists, HZO and Al 2O 3Two kinds of extraction agents can be used for extracting with IO 3 -The iodine that ionic species exists.Further studies show that extraction agent HZO and Al 2O 3Mo is also adsorbed, and Al 2O 3Absorption and desorption performance to Mo and I are suitable, and HZO is suitable to the absorption property of Mo and I, but relatively poor to the desorption performance of Mo.The results are shown in Table 2.
Table 2 HZO and Al 2O 3Respectively to molybdenum and iodine absorption and desorb test-results
Figure 2007103060555A00800061
From table 2 data as can be known, Al 2O 3Can be used for extracting simultaneously Mo and I, HZO can be used for extracting separately I.On the low side because of HZO to Mo absorption back desorption efficiency, be not suitable for and extract Mo.
Use Al 2O 3When post is done test, with the NH of different concns 3H 2O and NaOH solution stripping molybdenum and iodine the results are shown in Table 3 and table 4.
Table 3 NH 3H 2O concentration is to the influence (Al of molybdenum iodine desorption efficiency 2O 3Post)
Figure 2007103060555A00800062
Table 4 NaOH concentration is to the influence (HZO post) of molybdenum iodine desorption efficiency
From table 4 and table 5 data as can be known, use 0.5-2.0mol NH 3.H 2O desorb Al 2O 3Molybdenum and iodine on the post are better.Better with molybdenum and iodine on the 0.2-0.5mol/LNaOH desorb HZO post.
With HZO or Al 2O 3Exchange column is from UO 2(NO 3) 2Solution is that the uniform water solution nuclear reactor fuel solution of nuclear fuel extracts iodine and all must separate and remove Mo, owing to HZO or Al 2O 3Can both quantitatively adsorb IO 3 -The iodine of form, and can not adsorb I -Therefore the iodine of form can use an amount of reductive agent (as Na the iodine that extracts from reactor fuel solution and the mixture solution acidifying (as using HCl) of molybdenum then 2SO 3Perhaps Na 2S 2O 4), with IO 3 -Be reduced to I -, again through the height with diameter than being HZO purification column or the Al of 2-6 (being preferably 3-5) 2O 3Purification column absorption MoO 4 -, effluent is a NaI solution, this solution is Na 131The I product if effluent liquid purity is not enough, also can get the finished product through being further purified (another root purification column or conventional distillation method).Absorption MoO 4Purification column (the same extraction column of processing parameter), desorb MoO again after cleaning 4 -(processing parameter is with extraction column desorption technique parameter).Use Al 2O 3Extraction column and purification column extract the concrete extraction separation flow process and the correlation parameter of purifying iodine and molybdenum simultaneously and see Fig. 1.
Utilize Fig. 1 flow process Al 2O 3The experimental result that post extracts purifying iodine and molybdenum simultaneously sees Table 5, and the rate of recovery of iodine can reach 76.2%, and the rate of recovery of molybdenum can reach 57.9%.
Three Al of table 5 2O 3Post extracts purifying molybdenum and iodine experimental result simultaneously
Figure 2007103060555A00800071
Utilize 125I does separating of tracer agent simulation post III iodine and molybdenum, and schema is seen Fig. 2, after separating 125The contamination of I the results are shown in Table 6, and the result shows the Mo product through further evaporation calcination, and the Mo product can reach the pharmacopeia requirement.
In the table 6 post III molybdenum product 125The contamination experimental result of I
Figure 2007103060555A00800072
According to results of laboratory, prepared with UO 2(NO 3) 2Solution is the uniform water solution nuclear reactor fuel solution of nuclear fuel, carries out bench simulation test by 1: 1 scale, and extraction and purifying schema are seen Fig. 3.Extraction and separation simulation test-bed system schematic are seen Fig. 4.Fuel solution is UO 2(NO 3) 2-HNO 3Solution, wherein uranium concentration is 42.5mg/ML.HNO 3Concentration is 0.2mol/L, and the amount of the fission product element of preparation sees Table 7.
The add-on of element in table 7 bench simulation test
The rate of recovery of bench simulation test Mo and I sees Table 8, and the average recovery rate of Mo is 60.4%, and the average recovery rate of I is 50.6%.
The rate of recovery of table 8 bench testing Mo and I
Figure 2007103060555A00800082
The loss of bench simulation test U＜0.1%.This extraction and purifying process are fine to the fission product element decontamination that is added, and fail to detect the fission product element that is added in last iodine and the molybdenum product.Therefore the technology of extraction purifying iodine of the present invention can be used for from UO 2(NO 3) 2Solution is to extract purifying I-131 in the fuel solution of uniform water solution nuclear reactor of nuclear fuel, can obtain medical I-131 product, also can be used to extract purifying Mo-99 simultaneously, obtains medical Mo-99 product.

Claims (7)

1. extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor, it is characterized in that: this technology is adsorbed iodine-131 with aluminium sesquioxide extraction column or hydrous zirconium oxide extraction column the large volume fuel solution after reactor operation, uses rare HNO then successively 3, H 2O, NH 3H 2O cleans extraction column, uses NH again 3H 2Iodine-131 on O or the NaOH solution stripping extraction column carries out separation and purification to the iodine-131 after the desorb at last.
2. extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor as claimed in claim 1, it is characterized in that: the volume of aluminium sesquioxide extraction column or hydrous zirconium oxide extraction column is for extracting 1/100～1/50 of feed liquid, and the height of extraction column and diameter ratio are 2～6; Extraction column is before use through the presaturation of 0.1～0.3mol/L of 3.5～7 times of column volumes salpeter solution; The flow velocity of solution is 0.5～2.0ml/ml/min during absorption.
3. extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor as claimed in claim 1 or 2 is characterized in that: the scavenging solution that cleans extraction column is that the concentration of 3.5～7 times of column volumes is that the concentration of the water of 0.1～0.3mol/L nitric acid, 3.5～7 times of column volumes, 3.5～7 times of column volumes is the NH of 0.01mol/L 3H 2O; The flow velocity of three kinds of scavenging solutions is 0.5-2.0mL/mL/min.
4. extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor as claimed in claim 1 or 2 is characterized in that: during iodine-131 on the desorb extraction column, be 1～2mol/L NH with the concentration of 2.5～7 times of column volumes 3H 2O, desorb flow velocity are 0.5～2.0mL/mL/min; Perhaps the concentration with 2.5～7 times of column volumes is 0.2～1.0mol/LNaOH solution, and the desorb flow velocity is 0.5～2.0mL/mL/min.
5. extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor as claimed in claim 1 or 2 is characterized in that: the iodine-131 after the desorb is carried out separation and purification comprise the steps:
(1) stripping liquid of extraction column being adjusted to concentration of nitric acid with concentrated nitric acid is 0.1～0.3mol/L acidic medium, again by volume aluminium sesquioxide or the hydrous zirconium oxide purification column little than extraction column; The volume of purification column is to be purified 1/50～1/20 of feed liquid, and the height of purification column is 2～6 with the diameter ratio, through 3.5～7 times of column volume 0.1～0.3mol/L HNO 3Adsorb after the solution presaturation, the flow velocity of absorption iodine-131 is 0.5～2.0mL/mL/min again;
(2) be the HNO of 0.1～0.3mol/L with the concentration of 3.5～7 times of column volumes successively to the purification column behind the absorption iodine-131 3Solution, the H of 3.5～7 times of column volumes 2O, the concentration of 2.5～7 times of column volumes is 0.01mol/L NH 3H 2O solution cleans, and the flow velocity of three kinds of scavenging solutions is 0.5-2.0mL/mL/min;
(3) be 1～2mol/L NH with 2.5～7 times of column volume concentration 3H 2O is from aluminium sesquioxide purification column desorb iodine-131, or with the concentration of 2.5～7 times of column volumes be 0.2～1.0mol/L NaOH from hydrous zirconium oxide purification column desorb iodine-131, the desorb flow velocity is 0.5-2.0mL/mL/min.
6. extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor as claimed in claim 5 is characterized in that: as the Na from the purification column desorb 131I solution or NH 4 131Contain in the I solution 99MoO 4 -During negative ion impurity, the stripping liquid of regulating purification column with HCl is used Na again to acid 2SO 3Or Na 2S 2O 4Will 131IO 3 -Be reduced to 131I -, by second aluminium sesquioxide or hydrous zirconium oxide purification column, the concentration with 3.5～7 times of column volumes is 0.1～0.3mol/L HNO then again 3Solution, the H of 3.5～7 times of column volumes 2O, 3.5～7 times of column volume concentration are that 0.01mol/LNaOH solution cleans successively, the concentration with 2.5～7 times of column volumes is that 0.2～1.0mol/LNaOH solution stripping I-131 can get Na at last 131The I solution product, the desorb flow velocity is 0.5-2.0mL/mL/min.
7. extraction and purification technology of producing iodine-131 with uniform water solution nuclear reactor as claimed in claim 5 is characterized in that: when containing from the iodine-131 solution of purification column desorb 99MoO 4 -During negative ion impurity,, get Na at last with conventional distillation method purifying I-131 131The I solution product.
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US3998691A (en) * 1971-09-29 1976-12-21 Japan Atomic Energy Research Institute Novel method of producing radioactive iodine
CN1676461A (en) * 2003-09-10 2005-10-05 陈肖虎 Method for extracting iodine from rejected material generated during production of phosphor product from iodine-containing phosphorus ore
CN1794360A (en) * 2004-12-21 2006-06-28 韩国原子力研究所 Internal circulating irradiation capsule for iodine-125 and method of producing iodine-125 using same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3998691A (en) * 1971-09-29 1976-12-21 Japan Atomic Energy Research Institute Novel method of producing radioactive iodine
CN1676461A (en) * 2003-09-10 2005-10-05 陈肖虎 Method for extracting iodine from rejected material generated during production of phosphor product from iodine-containing phosphorus ore
CN1794360A (en) * 2004-12-21 2006-06-28 韩国原子力研究所 Internal circulating irradiation capsule for iodine-125 and method of producing iodine-125 using same

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