CN108977658B - A kind of Ni-63 solution γ nucleic minimizing technology - Google Patents
A kind of Ni-63 solution γ nucleic minimizing technology Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a kind of Ni-63 solution γ nucleic minimizing technologies, comprising: suitable anti-carrier is added into solution to be separated, and solution is switched to the system for being suitable for post separation, obtains sample solution, γ removal rate is improved by anti-carrier method.Second step, a post separation: anion exchange resin is used, strong γ nucleic in Ni-63 crude product, the Ni-63 sample solution Y2 after obtaining first separation are removed by the concentration and dosage of Non-leaching liquid, first separation γ removal rate is up to 99.96%.In order to further improve the purity of Ni-63 product solution, secondary separation can be carried out.Using this programme, secondary separation will be directly carried out after the resin column regeneration after first separation, obtain final Ni-63 product solution Y4, total γ removal rate is up to 99.999%；Success prepares high-purity63NiCl2Solution has established technical foundation for the preparation and measurement in the source Ni-63 β, while implementation cost is low.
Description
Technical field
The present invention relates to nucleic purifying technology fields, more particularly to a kind of Ni-63 solution γ nucleic minimizing technology.
Background technique
63Ni (Ni-63) half-life period is 100.1, can generate pure beta ray, ceiling capacity 66.9KeV, is at present in the world
One of most widely used low energy radiator beta-ray, reference source and operation source when can be used for β activity measurement and β energy response scale,
Chromatograph electron capture organ, ion smoke detector, electron capture probe of ionization source, gas chromatography etc. is multiple in electron tube answers
Use field.And63The production of Ni is to pass through62Ni occurs in reactor through neutron irradiation62Ni(n,γ)63It is obtained after Ni, then again
By separating-purifying, it is made high-purity63NiCl2Solution.And obtained after irradiating63In Ni crude product solution, except there are a large amount of nickel (packets
It includes63Ni product) outside, there is also certain radioactivity and on-radiation impurity, wherein60Co、58Co、57Co、59Fe etc. will be generated by force
Gamma-rays.According to EJ/T651-1992 standard pair63The requirement of the source Ni gamma activity limit value, final63HPGe γ in Ni solution product
The γ impurity of E γ > 100keV should be less than 0.1% in spectrometer detection, therefore, it is necessary to carry out separating-purifying to primary product, as far as possible
Remove strong γ nucleic therein.
In addition, nickel is widely used in reacting in pile element as metal material, activation products are also common in reactor
In the radioactive solid waste and waste water of generation, and63Ni as pure beta activity nucleic, be primarily present in aluminium alloy, stainless steel,
It is one of the critical nuclide for needing to detect in reactor decommissioning sample in the pile materialses such as graphite, concrete and lead.Therefore,
In the system63The accurate measurement of Ni activity is of great significance.But what it is due to the transmitting of β nucleic is continuous spectrum, in solid sample
In have serious self-absorption, and63The ray energy that Ni is emitted is lower, must be complete with other interference nucleic before measurement
Separation, therefore63The measurement of Ni is more demanding for Chemical Decomposition sample preparation program.
Either63The preparation of Ni isotope is still reacted in pile element63The measurement of Ni is required to remove in sample first
Strong γ nucleic.63NiCl2γ nucleic goes generally to use strongly basic anionic resin in solution, reaches removal by ion exchange
The purpose of γ nucleic.Although having similar research early period, mostly without experimental verification, system under strong γ radiation parameter
Separating property also need further to verify；And part resin price is expensive, is not suitable for industrial application.In addition, individual reports
The research that road has natural Ni target piece of the use in CARR research reactor after irradiation to carry out separation system, but due to62Ni(n,γ)63The reaction cross-section Ni is small, in natural Ni62Ni content is only 3.6345%, and irradiation is also only 10 days, generation63Ni specific activity is very
Low, the γ impurity content of generation is few, studies still in the laboratory proofing primary stage, application verification is insufficient.
It would therefore be highly desirable to establish a kind of method of good separating effect to solve63The efficient removal problem of γ nucleic in Ni solution.
Summary of the invention
It is solved for a kind of method for urgently establishing good separating effect set forth above63γ nucleic is efficient in Ni solution
The problem of removal problem, the present invention provides a kind of Ni-63 solution γ nucleic minimizing technology, this method passes through ion-exchange,
Provide a kind of method that can effectively remove γ nucleic in Ni-63 solution.
To solve the above problems, a kind of Ni-63 solution γ nucleic minimizing technology provided by the invention is wanted by following technology
Point is to solve the problems, such as: a kind of Ni-63 solution γ nucleic minimizing technology, including swivel is step S1 and post separation step S2；
The swivel is step S1 are as follows:
S1-1, cobalt carrier is added into sample solution, so that the total concentration of cobalt is 80~120 in finally obtained solution Y1
μg/mL；
S1-2, solution Y2 preparation: solution Y1 is heated, obtains solid after being evaporated；
After the solid is cooled to room temperature, concentration is used to be dissolved for the hydrochloric acid of 10~12mol/L, so that final molten
The concentration of nickel obtains solution Y2 less than 5000 μ g/mL in liquid；
The post separation step S2 are as follows:
The pretreatment of S2-1, column: resin is that quaternary ammonium is had in styrene-divinylbenzene copolymer of gel cross-linkage structure
Base [- N (CH3)3OH] anion exchange resin, using 30~60min of salt acid soak anion exchange resin of 3~5mol/L
Upper prop afterwards, then uses the hydrochloric acid leaching resin column of 3~5mol/L, and the resin of every 10ML is eluted using the hydrochloric acid of 30~50ML；
Resin column then is eluted with 2%~5% sodium hydroxide solution again, the resin of every 10mL is molten using the sodium hydroxide of 30~50mL
Liquid elution；Finally resin column is eluted to neutrality with deionized water；
S2-2, separation: the resin column obtained using 10~12mol/L hydrochloric acid rinsing step S2-1, the body of the hydrochloric acid of addition
Product is 3~5 times of the resin volume of dress column；Then solution Y2 is added in resin column, after solution drains off just in column, then is used
10~12mol/L hydrochloric acid leaching resin column, the volume that hydrochloric acid leacheate is added is 1~3 times of Y2 solution, by resin column outflow
Liquid is the Ni-63 solution for eliminating γ nucleic.
In the present solution, the upper prop is that will carry out resin column preparation through the anion exchange resin that persalt impregnates.It is preferred that
Pillar ratio of height to diameter that post separation uses being set as 10:1~60:1, the volume of separation resin needed for every 1g nickel is 100~
500mL。
Further technical solution are as follows:
When the resin column of Y2 solution was added using 10~12mol/L hydrochloric acid rinsing step S2-2, it is small that hydrochloric acid elutes speed
In or equal to 0.8mL/min.
In step S2-2, introduced liquid is eluted by hydrochloric acid is no longer flowed out in resin column in solution Y2 addition resin column
Shi Jinhang；
The more changing-over liquid bottle when solution Y2 to be added in resin column.
Complete solution Y2 be added resin column in and resin column there is no fluid flow out when, to resin column be added 10~
12mol/L hydrochloric acid continues to elute resin column, and the volume that hydrochloric acid leacheate is added is 1~3 times of the Y2 liquor capacity being added, at this time
Liquid bottle is connect to continue to collect liquid.
It further include repeated removal step, the repeated removal step includes the repetition swivel system and repeat column point that sequence carries out
From the swivel system that repeats is that Ni-63 solution resulting to step S2-2 does following processing:
Cobalt carrier is added into Ni-63 solution, so that the total concentration of cobalt is 80~120 in acquired solution Y3
μg/mL；
The above solution Y3 is heated, obtains solid after being evaporated；
After the solid as described in solution Y3 is cooled to room temperature, uses concentration to be dissolved for the hydrochloric acid of 10~12mol/L, make
The concentration of nickel in final solution is obtained less than 5000 μ g/mL, obtains solution Y4；
It is described to repeat post separation are as follows:
Use resin column to be separated: resin in the styrene of gel cross-linkage structure-divinylbenzene copolymer have season
Ammonium [- N (CH3)3OH] anion exchange resin.
The post separation that repeats includes resin column regeneration and secondary post separation:
The resin column regeneration are as follows: following processing is done to used resin column in this method implementation process: to resin column
Middle addition deionized water, cobalt remaining in resin column is eluted, and the volume that deionized water is added is the Y2 solution being added
5~8 times of volume；And the hydrochloric acid leaching resin column of 10~12mol/L is added in backward resin column, the hydrochloric acid leacheate of addition
Volume is 3~5 times of the resin volume of dress column；Resin column each region is then made to be infiltrated on the hydrochloric acid of 10~12mol/L
For protecting column；
The secondary post separation are as follows: resin column switch is opened, after hydrochloric acid remaining in resin column regenerative process drains off, to
Solution Y4 and more changing-over liquid bottle is added in resin column, after solution drains off just in column, then with 10~12mol/L hydrochloric acid leaching resin
Column, the volume that hydrochloric acid leacheate is added is 1~3 times of Y4, and the liquid by resin column outflow is the Ni-63 for eliminating γ nucleic
Solution.
The repeated removal step includes the multiple of sequence progress, and the raw material of first time repeated removal step is step
The resulting Ni-63 solution of S2-2, the raw material of subsequent repeated removal step are that the resulting Ni-63 of last repeated removal step is molten
Liquid.
The invention has the following advantages:
Using this programme, can efficiently remove in Ni-63 solution strong γ nucleic (60Co、58Co、57Co、59Fe), primary point
Overall recovery from rear nickel is up to 95%；
This programme carries out the removal of strong γ nucleic using anti-carrier method, is remarkably improved the removal rate of γ nucleic: implementing this
Scheme, total γ activity is 4.86 × 10 before gamma ray spectrometer measures separation8Bq after secondary separation, that is, implements a repeated removal step
Afterwards, total γ activity is then 857Bq, and the removal rate of total γ nucleic may be up to 99.999%.
The resin that this programme uses is at low cost and reusable.
Detailed description of the invention
Fig. 1 is separation curve graph described in embodiment 1, which is 12mol/L HCl, 500mg/L Ni2+、
Co2+Under the conditions of separation curve.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, but the present invention is not limited only to following implementation
Example:
Embodiment 1:
Present embodiments provide a kind of concrete implementation mode:
In the present embodiment, experimental water is deionized water, and is used after Quartz Sub-Boiling Distiller distills, resistivity >
18MΩ.cm。
Specific step is as follows:
The first step, primary swivel system:
The addition of 1.1 anti-carrier cobalts.
Cobalt standard solution 1mL is accurately pipetted in 5mL Ni-63 solution to be separated with 1mL liquid-transfering gun.The Ni-63 solution
In nickel concentration be about 500 μ g/mL, obtain sample solution Y1.Anti-carrier cobalt carrier needed for all steps is validity period in experiment
Within cobalt standard solution, concentration is 1000 μ g/mL, and opposite expanded uncertainty is 0.7%, k=2.
The preparation of 1.2 sample lysate Y2.
Solution Y1 is placed on electric hot plate, middle-grade is heated to just absolutely dry.After sample is cooling, graduated cylinder measures 10mL's
12mol/L hydrochloric acid is added in sample, is placed half angel's solid and is all dissolved, obtains the sample solution of yellow green clear,
Sample solution Y2 is obtained, wherein cobalt concentration is about 100 μ g/mL.
Second step, a post separation:
The pretreatment of 2.1 columns.
The resin that post separation uses is in styrene-divinylbenzene copolymer of gel cross-linkage structure with quaternary ammonium group [- N
(CH3)3OH] nuclear leve anion exchange resin, brand ZGANR170.Splitter is Φ 10mm, long 30cm, glass material.Dress
Using upper prop after 3mol/L salt acid soak anion exchange resin 30min before column, pillar height is controlled in 13cm, the resin volume of addition
For 10mL.Dress column after the completion of use 50mL 3mol/L hydrochloric acid leaching resin column, after again with 5% sodium hydroxide solution of 50mL drench
Resin column is washed, finally resin column is eluted to neutrality with deionized water, it is stand-by to protect column.
2.2 post separation detailed processes.
50mL 12mol/L hydrochloric acid leaching resin column is used before sample upper prop, adjusting makes flow velocity 08mL/min, lucky to hydrochloric acid
Solution Y2 to be separated is added in resin column after draining off, while more changing-over liquid bottle, is mended after sample liquid drains off just with graduated cylinder
Add the 12mol/L hydrochloric acid of 26mL to continue to elute resin column, drains off just to solution in column and close resin column switch, the solution connect
As Ni-63 sample.
Third step, secondary swivel system:
The addition of 3.1 anti-carrier cobalts.
The cobalt standard solution of 1mL is accurately added in the step resulting Ni-63 sample of post separation with 1mL liquid-transfering gun upwards,
Sample solution Y3 is obtained, anti-carrier cobalt carrier used in experiment is the cobalt standard solution within validity period, and cobalt standard solution is dense
Degree is 1000 μ g/mL, opposite expanded uncertainty is 0.7%, k=2.
The preparation of 3.2 sample lysate Y4.
The sample solution after anti-carrier will be added to be placed on electric hot plate, it is just absolutely dry that middle-grade is heated to solution, cold to sample
But the 12mol/L hydrochloric acid of 10mL is accurately added by graduated cylinder afterwards, placement dissolves solid all, obtains yellow green clear
Sample solution Y4, wherein cobalt concentration is about 100 μ g/mL.
4th step, secondary post separation:
The regeneration of 4.1 resin columns.
Since resin column is reusable, 60mL deionized water is added in the resin column after Xiang Yici post separation, more renews
Connect liquid bottle, coutroi velocity 1.2mL/min elutes cobalt remaining in resin column, proper to the deionized water in resin column
After draining off well, what is more renewed connects liquid bottle；50mL 12mol/L hydrochloric acid leaching resin column is added into the resin column, adjusting makes flow velocity
0.8mL/min, last residue 5mL hydrochloric acid protect column and complete the regeneration of resin column for use.
4.2 2 post separation detailed processes.The switch of resin column is opened, coutroi velocity 0.8mL/min, to be remained in column
Remaining hydrochloric acid upper sample solution Y4 after draining off just, at the same replace it is clean connect liquid bottle, add 30mL after sample liquid drains off just
12mol/L hydrochloric acid continue elute resin column, drain off to solution in column, the solution connect is Ni-63 product solution.
For the above specific implementation step, the γ nucleic removal rate in nickel purification process is as shown in the table:
γ nucleic removal rate in nickel purification process
Can be obtained by above table: using this method, corresponding resin system is fabulous to nickel, cobalt separating effect.
For the above specific embodiment, obtain separating curve as shown in Figure 1.
About the separation curve that Fig. 1 is provided, abscissa is the effluent volume of resin column in figure, after upper sample solution Y2
Start to count, which includes three parts, and first part is sample solution Y2, and second part is added after sample solution drains off
The hydrochloric acid leacheate of the 10-12mol/L entered, Part III are the deionized waters for rinsing cobalt in column.
Ordinate respectively indicates the concentration of nickel in the efflux of this resin column, cobalt.Concrete operations are in experiment: upper sample
It after solution Y2, often fills 5mL sample and just replaces and once connect liquid bottle, until last deionized water drains off just, generate a large amount of samples
Product are measured nickel, the cobalt concentration in each sample by elution order, depict this separation curve graph.As seen from the figure, exist
In first more than 20 milliliters of volume, nickel is largely to flow out, and the concentration of cobalt is background in this part abscissa, and basic holding is not
Become.After it joined deionized water elution below, cobalt ions largely flows out.The peak of nickel and the peak of cobalt are completely separable, also with regard to table
The separation for successfully realizing nickel, cobalt is illustrated, and system is fine to the separating degree of nickel, cobalt.In addition, also show when only with 10~
The hydrochloric acid leaching resin column of 12mol/L, cobalt are will not to be leached substantially；And deionized water can quickly elute down cobalt
Come, it is easy to accomplish the regeneration of resin column.
The above content is combine specific preferred embodiment to the further description of the invention made, and it cannot be said that originally
The specific embodiment of invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs,
The other embodiments obtained in the case where not departing from technical solution of the present invention, should be included within the scope of the present invention.
Claims (7)
1. a kind of Ni-63 solution γ nucleic minimizing technology, which is characterized in that including swivel be step S1 and post separation step S2；
The swivel is step S1 are as follows:
S1-1, cobalt carrier is added into sample solution, so that the total concentration of cobalt is 80~120 μ g/ in finally obtained solution Y1
mL；
S1-2, solution Y2 preparation: solution Y1 is heated, obtains solid after being evaporated；
After the solid is cooled to room temperature, concentration is used to be dissolved for the hydrochloric acid of 10~12mol/L, so that in final solution
The concentration of nickel obtains solution Y2 less than 5000 μ g/mL；
The post separation step S2 are as follows:
The pretreatment of S2-1, column: the pillar ratio of height to diameter that post separation uses for 10:1~60:1, separation resin needed for every 1g nickel
Volume is 100~500mL；Resin is that quaternary ammonium group [- N is had in styrene-divinylbenzene copolymer of gel cross-linkage structure
(CH3)3OH] anion exchange resin, on after 30~60min of salt acid soak anion exchange resin of 3~5mol/L
Column, then uses the hydrochloric acid leaching resin column of 3~5mol/L, and the resin of every 10ML is eluted using the hydrochloric acid of 30~50ML；Then
Resin column is eluted with 2%~5% sodium hydroxide solution again, the resin of every 10mL is drenched using the sodium hydroxide solution of 30~50mL
It washes；Finally resin column is eluted to neutrality with deionized water；
S2-2, separation: the resin column obtained using 10~12mol/L hydrochloric acid rinsing step S2-1, the volume of the hydrochloric acid of addition are
Fill 3~5 times of the resin volume of column；Then solution Y2 is added in resin column, after solution drains off just in column, then with 10~
12mol/L hydrochloric acid leaching resin column, the volume that hydrochloric acid leacheate is added is 1~3 times of Y2 solution, the liquid flowed out by resin column
As eliminate the Ni-63 solution of γ nucleic.
2. a kind of Ni-63 solution γ nucleic minimizing technology according to claim 1, which is characterized in that using 10~
When the resin column of Y2 solution was added in 12mol/L hydrochloric acid rinsing step S2-2, hydrochloric acid elutes speed and is less than or equal to 0.8mL/
min。
3. a kind of Ni-63 solution γ nucleic minimizing technology according to claim 2, which is characterized in that in step S2-2,
Introduced liquid when progress is eluted by hydrochloric acid is no longer flowed out in resin column in solution Y2 addition resin column；
The more changing-over liquid bottle when solution Y2 to be added in resin column.
4. a kind of Ni-63 solution γ nucleic minimizing technology according to claim 3, which is characterized in that complete solution Y2
It is added in resin column and resin column is there is no when fluid outflow, 10~12mol/L hydrochloric acid is added to resin column and continues to elute resin
Column, the volume that hydrochloric acid leacheate is added is 1~3 times of the Y2 liquor capacity being added, connects liquid bottle at this time and continues to collect liquid.
5. a kind of Ni-63 solution γ nucleic minimizing technology according to claim 1, which is characterized in that further include repeating to go
Except step, the repeated removal step includes the repetition swivel system and repeat post separation that sequence carries out, and the swivel system that repeats is
Ni-63 solution resulting to step S2-2 does following processing:
Cobalt carrier is added into Ni-63 solution, so that the total concentration of cobalt is 80~120 μ g/mL in acquired solution Y3；
The above solution Y3 is heated, obtains solid after being evaporated；
After the solid as described in solution Y3 is cooled to room temperature, concentration is used to be dissolved for the hydrochloric acid of 10~12mol/L, so that most
The concentration of nickel obtains solution Y4 less than 5000 μ g/mL in whole solution；
It is described to repeat post separation are as follows:
Use resin column to be separated: resin in the styrene of gel cross-linkage structure-divinylbenzene copolymer have quaternary ammonium group
[-N(CH3)3OH] anion exchange resin.
6. a kind of Ni-63 solution γ nucleic minimizing technology according to claim 5, which is characterized in that described to repeat column point
From including resin column regeneration and secondary post separation:
The resin column regeneration are as follows: following processing is done to used resin column in this method implementation process: being added into resin column
Enter deionized water, cobalt remaining in resin column is eluted, the volume that deionized water is added is the Y2 liquor capacity being added
5~8 times；And the hydrochloric acid leaching resin column of 10~12mol/L is added in backward resin column, the volume of the hydrochloric acid leacheate of addition
It is 3~5 times of the resin volume of dress column；Then make resin column each region be infiltrated on the hydrochloric acid of 10~12mol/L with
Yu Baozhu；
The secondary post separation are as follows: resin column switch is opened, after hydrochloric acid remaining in resin column regenerative process drains off, to resin
Solution Y4 and more changing-over liquid bottle is added in column, after solution drains off just in column, then with 10~12mol/L hydrochloric acid leaching resin column,
The volume that hydrochloric acid leacheate is added is 1~3 times of Y4, and the Ni-63 for as eliminating γ nucleic by the liquid of resin column outflow is molten
Liquid.
7. a kind of Ni-63 solution γ nucleic minimizing technology according to claim 5, which is characterized in that the repeated removal
Step includes the multiple of sequence progress, and the raw material of first time repeated removal step is the resulting Ni-63 solution of step S2-2, after
The raw material of continuous repeated removal step is the resulting Ni-63 solution of last repeated removal step.
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| CN113413928B (en) * | 2021-06-23 | 2023-04-21 | 中国核动力研究设计院 | Nickel-63 automatic separation device and separation process thereof |
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|---|---|
| CN108977658A (en) | 2018-12-11 |
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