CN112403032A - In homogeneous water solution nuclear reactor fuel solution99Mo、131I co-extraction method - Google Patents
In homogeneous water solution nuclear reactor fuel solution99Mo、131I co-extraction method Download PDFInfo
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- 238000000658 coextraction Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910001868 water Inorganic materials 0.000 title claims abstract description 9
- 239000003758 nuclear fuel Substances 0.000 title claims description 16
- 239000000243 solution Substances 0.000 claims abstract description 94
- 238000000605 extraction Methods 0.000 claims abstract description 35
- 239000000446 fuel Substances 0.000 claims abstract description 31
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 7
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000004140 cleaning Methods 0.000 claims description 31
- 238000003795 desorption Methods 0.000 claims description 21
- 239000000945 filler Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052770 Uranium Inorganic materials 0.000 abstract description 12
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 description 17
- 229910052740 iodine Inorganic materials 0.000 description 11
- 229910052750 molybdenum Inorganic materials 0.000 description 11
- 238000001179 sorption measurement Methods 0.000 description 10
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000011630 iodine Substances 0.000 description 5
- 238000002386 leaching Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- ZOKXTWBITQBERF-AKLPVKDBSA-N Molybdenum Mo-99 Chemical compound [99Mo] ZOKXTWBITQBERF-AKLPVKDBSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 3
- 229950009740 molybdenum mo-99 Drugs 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- 229910000384 uranyl sulfate Inorganic materials 0.000 description 2
- PNDPGZBMCMUPRI-HVTJNCQCSA-N 10043-66-0 Chemical compound [131I][131I] PNDPGZBMCMUPRI-HVTJNCQCSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- VANPZBANAIIRJW-UHFFFAOYSA-N diuranium Chemical compound [U]#[U] VANPZBANAIIRJW-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
- B01D15/426—Specific type of solvent
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a homogeneous aqueous solution in fuel solution of nuclear reactor99Mo、131I Co-extraction method, the cooled fuel solution is absorbed by a spherical alumina extraction column99Mo and131i, sequentially washing the extraction column with nitric acid, water and ammonia water, desorbing the extraction column with ammonia water or sodium hydroxide solution, and purifying99Mo and131i is desorbed to realize99Mo and131and (I) co-extraction. The invention is suitable for high-concentration uranium fuel solution99Mo and131i co-extraction, also applicable to low-enriched uranium fuel solution99Mo and131i, co-extracting the raw materials,99mo and131the extraction rate of I is more than 80%.
Description
Technical Field
The invention relates to a production technology of medical radionuclide, in particular to a method for preparing homogeneous aqueous solution in nuclear reactor fuel solution99Mo、131I method of co-extraction.
Background
Molybdenum-99 (99Mo) and iodine-131 (131I) Are two important medical radioactive isotopes.99Mo and131the traditional production method of I is a target irradiation method. Nuclear reactors using aqueous solutions of uranyl nitrate (or uranyl sulfate) as nuclear fuel were proposed in the last 90 s of the century for use in nuclear reactors99Mo and131and (I) producing. Homogeneous aqueous solution nuclear reactor production99Mo and131in uranyl nitrate (or uranyl sulfate) at I235U timely reactor operation fuel and simultaneously generation99Mo and131the production process of "target material" of medical radioactive isotope, such as I, also omits the procedures of making target and solution, etc., so that compared with target irradiation method it can produce homogeneous aqueous solution by nuclear reactor99Mo and131the method has the advantages of high neutron utilization rate, less waste generation amount, simple and convenient process, low operation cost and the like, and has obvious advantages.
The existing three alumina columns are used for extraction and separation in high-concentration uranium (uranium)235U abundance of 90%) in uranyl nitrate solution,99recovery rate of MoThe content of the active carbon reaches 56.4 percent,131the recovery rate of I reaches 50.6%. But in low enriched uranium: (235U abundance less than 20%) in the fuel solution,99mo and131the extraction rate of I is greatly reduced. In recent years, there has been a trend towards the promotion and use of low enriched uranium fuels in nuclear-related processes in order to reduce the risk of nuclear diffusion and terrorist events. Therefore, there is a need to develop new extraction processes to improve the fuel solution99Mo and131extraction yield of I, especially low enriched uranium: (235U abundance less than 20%) in fuel solution99Mo and131the extraction rate of I and the economic benefit are improved.
Disclosure of Invention
The present invention has been made to solve the above-mentioned problems occurring in the prior art, and provides a method for co-extracting 99Mo and 131I from a homogeneous aqueous solution nuclear reactor fuel solution, which can be implemented in a fuel solution containing a large amount of fission products99Mo、131The co-extraction of I can be realized in a high-concentration uranium fuel solution99Mo and131i co-extraction can also be realized in low-enriched uranium fuel solution99Mo and131i co-extracting as follows99Mo、131I is prepared for isolation and purification.
The invention is realized by the following technical scheme:
in homogeneous water solution nuclear reactor fuel solution99Mo、131I Co-extraction method, the cooled fuel solution is absorbed by a spherical alumina extraction column99Mo and131I。
the method comprises the following specific steps: adsorbing the cooled fuel solution by a spherical alumina extraction column99Mo and131i, sequentially washing the extraction column with nitric acid, water and ammonia water, desorbing the extraction column with ammonia water or sodium hydroxide solution, and purifying99Mo and131i is desorbed to realize99Mo and131and (I) co-extraction.
Furthermore, the specific surface area of the filler spherical alumina in the extraction column is 100-300 m2/g。
Furthermore, the grain diameter of the filler spherical alumina in the extraction column is 40-200 μm.
Furthermore, the ratio of the height to the diameter of the extraction column is 2-8.
Furthermore, the concentration of the nitric acid cleaning solution is 0.01-1.0 mol/L, the volume of the nitric acid cleaning solution is 2-10 times of the volume of the extraction column, and the cleaning flow rate is 0.04-1.0 mL/mL of column packing/min.
Furthermore, the volume of the water washing liquid is 2-10 times of the volume of the extraction column, and the washing flow rate is 0.04-1.0 mL/min of column packing.
Furthermore, the concentration of the ammonia water cleaning solution is 0.001-0.05 mol/L, the volume of the ammonia water cleaning solution is 2-10 times of the volume of the extraction column, and the cleaning flow rate is 0.04-1.0 mL/mL of column packing/min.
Furthermore, the concentration of desorption liquid ammonia water or sodium hydroxide solution is 0.2-2.0 mol/L, the volume is 2-10 times of the volume of the extraction column, and the desorption flow rate is 0.04-1.0 mL/mL of column packing/min.
The invention has the following beneficial effects:
the invention relates to a homogeneous aqueous solution in the fuel solution of a nuclear reactor99Mo、131The method of I co-extraction is not only suitable for the high-concentration uranium fuel solution99Mo and131i co-extraction, also applicable to low-enriched uranium fuel solution99Mo and131i, co-extracting the raw materials,99mo and131the extraction rate of I is more than 80 percent, and the method can be used for the production of homogeneous aqueous solution nuclear reactors99Mo and131I。
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1
The invention relates to a homogeneous aqueous solution in the fuel solution of a nuclear reactor99Mo、131I the method of co-extraction, 2g of activated spherical alumina is respectively weighed and packed into columns with the height-diameter ratio of 2, 4, 6 and 8 respectively. After the pretreatment with 0.1mol/L nitric acid solution is finished, adding U concentrate50mL of fuel solution containing 1mg/L of molybdenum and 2mg/L of iodine is loaded on the column for adsorption, and the concentration is 50 g/L. After the adsorption is finished, sequentially adding 0.1mol/L HNO3And (3) cleaning the solution, deionized water and 0.001mol/L ammonia water, wherein the volume of the cleaning solution is 2 times of the volume of the column to drip the spherical alumina column, and the flow rate of the cleaning solution is 0.1mL/mL of column filler/min. After leaching is finished, desorbing the spherical alumina column by 0.2mol/L ammonia water, wherein the volume of the desorption liquid is 10 times that of the column, and the flow rate of the desorption liquid is 0.1mL/mL of column filler/min. The measured recovery rate of U is more than 99.99 percent, the recovery rate of Mo is 91.6 to 97.6 percent, and the recovery rate of I is 89.3 to 96.2 percent (see table 1).
TABLE 1 Co-extraction Effect of Mo and I by different column height-diameter ratios
Example 2:
the invention relates to a homogeneous aqueous solution in the fuel solution of a nuclear reactor99Mo、131I the co-extraction method, 2g of activated spherical alumina is weighed and packed into columns with the height-diameter ratio of 4 respectively. After the pretreatment with 0.1mol/L nitric acid solution is finished, 50mL of fuel solution containing 1mg/L molybdenum and 2mg/L iodine and with the U concentration of 50g/L is added to the column for adsorption. After the adsorption is finished, sequentially adding 0.1mol/L HNO3And (3) cleaning the solution, deionized water and 0.001mol/L ammonia water, wherein the volume of the cleaning solution is 2 times of the volume of the column to drip the spherical alumina column, and the flow rate of the cleaning solution is 0.1mL/mL of column filler/min. After leaching, desorbing the spherical alumina column by using 0.2mol/L ammonia water, wherein the volume of the desorption liquid is 10 times that of the column, and the flow rates of the desorption liquid are 0.01, 0.1, 0.2 and 0.4mL/mL of column filler/min respectively. The measured recovery rate of U is more than 99.96 percent, the recovery rate of Mo is 89.4 to 98.3 percent, and the recovery rate of I is 88.6 to 97.5 percent (see table 2).
TABLE 2 Co-extraction effect of ammonia desorption solution on Mo and I at different flow rates
Example 3:
the invention relates to a homogeneous aqueous solution in the fuel solution of a nuclear reactor99Mo、131I the co-extraction method, 2g of activated spherical alumina is weighed and packed into columns with the height-diameter ratio of 4 respectively. After the pretreatment with 0.1mol/L nitric acid solution is finished, 50mL of fuel solution containing 1mg/L molybdenum and 2mg/L iodine and with the U concentration of 50g/L is added to the column for adsorption. After the adsorption is finished, sequentially adding 0.1mol/L HNO3And (3) cleaning the solution, deionized water and 0.001mol/L ammonia water, wherein the volume of the cleaning solution is 2 times of the volume of the column to elute the spherical alumina column, and the cleaning solution is 0.1mL/mL of column filler/min. After leaching, desorbing the spherical alumina column by using 0.2, 0.5, 1.0 and 2.0mol/L ammonia water respectively, wherein the volume of the desorption liquid is 10 times that of the column, and the flow rate of the desorption liquid is 0.1mL/mL of column filler/min. The measured recovery rate of U is more than 99.98 percent, the recovery rate of Mo is 93.5 to 98.5 percent, and the recovery rate of I is 92.1 to 97.3 percent (see table 3).
TABLE 3 Co-extraction effect of different concentrations of ammonia water desorption solution on Mo and I
Example 4:
the invention relates to a homogeneous aqueous solution in the fuel solution of a nuclear reactor99Mo、131I the co-extraction method, 2g of activated spherical alumina is weighed and packed into columns with the height-diameter ratio of 4 respectively. After the pretreatment with 0.1mol/L nitric acid solution is finished, 50mL of fuel solution containing 1mg/L molybdenum and 2mg/L iodine and with the U concentration of 50g/L is added to the column for adsorption. After the adsorption is finished, sequentially adding 0.1mol/L HNO3And (3) cleaning the solution, deionized water and 0.001mol/L ammonia water, wherein the volume of the cleaning solution is 2 times of the volume of the column to drip the spherical alumina column, and the flow rate of the cleaning solution is 0.1mL/mL of column filler/min. After leaching, desorbing the spherical alumina column with 0.2, 0.5, 1.0 and 2.0mol/L sodium hydroxide respectively, wherein the volume of the desorption liquid is 10 times that of the column, and the flow rate of the desorption liquid is 0.1mL/mL column packing/min. The measured recovery rate of U is more than 99.95%, the recovery rate of Mo is 97.4-99.9%, and the recovery rate of I is 96.2-99.4% (see table 4).
TABLE 4 Co-extraction Effect of different NaOH stripping solution concentrations on Mo and I
Example 5:
the invention relates to a homogeneous aqueous solution in the fuel solution of a nuclear reactor99Mo、131I the co-extraction method, 2g of activated spherical alumina is weighed and packed into columns with the height-diameter ratio of 4 respectively. After the pretreatment with 0.1mol/L nitric acid solution is finished, 50mL of fuel solution containing 1mg/L molybdenum and 2mg/L iodine and with the U concentration of 250g/L is added to the column for adsorption. After the adsorption is finished, sequentially adding 0.1mol/L HNO3And (3) cleaning the solution, deionized water and 0.001mol/L ammonia water, wherein the volume of the cleaning solution is 2 times of the volume of the column to drip the spherical alumina column, and the flow rate of the cleaning solution is 0.1mL/mL of column filler/min. After leaching is finished, desorbing the spherical alumina column by using 1mol/L ammonia water, wherein the volume of the desorption liquid is 10 times that of the column, and the flow rate of the desorption liquid is 0.1mL/mL of column packing/min. The measured recovery rate of U reaches 99.95%, the recovery rate of Mo is 87.4%, the recovery rate of I is 81.6%, and U is not detected in the desorption solution of Mo and I, so that the co-extraction of Mo and I is realized.
In conclusion, the experimental data show that99Mo、131The method of I co-extraction is not only suitable for the high-concentration uranium fuel solution99Mo and131i co-extraction, also applicable to low-enriched uranium fuel solution99Mo and131i, co-extracting the raw materials,99mo and131the extraction rate of I can reach more than 80%.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. In homogeneous water solution nuclear reactor fuel solution99Mo、131I co-extraction method is characterized in that cooled fuel solution is adsorbed by a spherical alumina extraction column99Mo and131I。
2. the homogeneous aqueous solution nuclear reactor fuel solution of claim 199Mo、131The method for I co-extraction is characterized by comprising the following specific steps: adsorbing the cooled fuel solution by a spherical alumina extraction column99Mo and131i, sequentially washing the extraction column with nitric acid, water and ammonia water, desorbing the extraction column with ammonia water or sodium hydroxide solution, and purifying99Mo and131i is desorbed to realize99Mo and131and (I) co-extraction.
3. The homogeneous aqueous solution nuclear reactor fuel solution of claim 199Mo、131The method for I co-extraction is characterized in that the specific surface area of filler spherical alumina in an extraction column is 100-300 m2/g。
4. The homogeneous aqueous solution nuclear reactor fuel solution of claim 199Mo、131The method for the co-extraction is characterized in that the grain diameter of filler spherical alumina in an extraction column is 40-200 mu m.
5. The homogeneous aqueous solution nuclear reactor fuel solution of claim 199Mo、131The method for the I co-extraction is characterized in that the ratio of the height to the diameter of an extraction column is 2-8.
6. The homogeneous aqueous solution nuclear reactor fuel solution of claim 299Mo、131I together withThe extraction method is characterized in that the concentration of the nitric acid cleaning solution is 0.01-1.0 mol/L, the volume of the nitric acid cleaning solution is 2-10 times of the volume of the extraction column, and the cleaning flow rate is 0.04-1.0 mL/mL of column packing/min.
7. The homogeneous aqueous solution nuclear reactor fuel solution of claim 299Mo、131The method for the co-extraction is characterized in that the volume of a water washing liquid is 2-10 times of the volume of an extraction column, and the washing flow rate is 0.04-1.0 mL/mL of column packing/min.
8. The homogeneous aqueous solution nuclear reactor fuel solution of claim 299Mo、131The method for I co-extraction is characterized in that the concentration of an ammonia water cleaning solution is 0.001-0.05 mol/L, the volume of the ammonia water cleaning solution is 2-10 times of the volume of an extraction column, and the cleaning flow rate is 0.04-1.0 mL/mL of column filler/min.
9. The homogeneous aqueous solution nuclear reactor fuel solution of claim 299Mo、131The method for I co-extraction is characterized in that the concentration of desorption liquid ammonia water or sodium hydroxide solution is 0.2-2.0 mol/L, the volume of the desorption liquid ammonia water or sodium hydroxide solution is 2-10 times of the volume of an extraction column, and the desorption flow rate is 0.04-1.0 mL/column filler/min.
10. The homogeneous aqueous solution nuclear reactor fuel solution of claim 299Mo、131The method for the co-extraction is characterized in that the ratio of the height to the diameter of an extraction column is 4; the concentration of the nitric acid cleaning solution is 0.1mol/L, the concentration of the ammonia water cleaning solution is 0.001mol/L, the volumes of the cleaning solutions are all 2 times of the column volume to drip the spherical alumina column, and the flow rates of the cleaning solutions are all 0.1mL/mL of column filler/min; the concentration of ammonia water in the desorption solution is 1mol/L, the volume of the desorption solution is 10 times of the volume of the column, and the flow rate of the desorption solution is 0.1 mL/column packing/min.
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