CN103589866A - Separation and recovery method for thorium and uranium by using silicon-based anion exchange resin - Google Patents
Separation and recovery method for thorium and uranium by using silicon-based anion exchange resin Download PDFInfo
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- CN103589866A CN103589866A CN201310627541.2A CN201310627541A CN103589866A CN 103589866 A CN103589866 A CN 103589866A CN 201310627541 A CN201310627541 A CN 201310627541A CN 103589866 A CN103589866 A CN 103589866A
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Abstract
The invention relates to a separation and recovery method for thorium and uranium by using a silicon-based anion exchange resin. The method comprises the following steps: dissolving a raw material containing radioactive elements like thorium and uranium in high concentration nitric acid to form a nitrate solution of thorium and uranium; adding the anion exchange resin into a nitric acid system mentioned above for ion exchange adsorption; and leaching thorium adsorbed on the anion exchange resin after completion of ion exchange so as to realize separation and recovery of thorium and uranium. According to the invention, the silicon-based anion exchange resin is employed for separation and recovery of thorium and uranium in raw materials like spent fuels of nuclear power stations; the method is simple and easy to operate, phase separation difficulty and solvent loss do not exist, and in particular, usage of a porous SiO2 carrier ensures stability of the method under high-acid strong-irradiation application conditions.
Description
Technical field
The invention belongs to the separation and recovery technology field of thorium, uranium element, particularly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery.
Background technology
232th, as the material that can be converted into nuclear fuel, is a kind of potential resources of Nuclear energy uses.Occurring in nature contains more rich
232th isotropic substance, its reserves are approximately 3 times of uranium resources.China is that a uranium ore resource is poorer, the more rich country and thorium reserves compare.
232th itself is not fissile material, in order to utilize thorium in nuclear energy engineering, need to incite somebody to action by a series of nuclear reactions
232th is transformed into fissile material
233u.These a series of nuclear reactions are carried out in reactor, easily fissile nucleus
235u or
239the neutron irradiation that Pu discharges in fission process
232th, makes it to be converted to easy fission
233u.Generate
233u enters circulation again and participates in fission, has just formed Th-U Fuel cycle.The object elements that needs most the reusable edible of recovery in thorium base spent fuel is Th and U, but Th-U Fuel cycle technique is still immature.In thorium base spent fuel in conceptual phase, also there is not efficient recovery method in Th-U separation and recovery method many places at present.In addition, from light-water reactor uranium oxide spent fuel, reclaim the uranium product obtain, contain trace (0.5～4ppb/U)
23272 years U(transformation period), its descendant
2281.9 years Th(transformation period) descendant generating through multistage further decay
21260.6 minutes Bi(transformation period) and
2083 minutes Ti(transformation period) can emit high-octane gamma-rays, have a strong impact on and reclaim uranium as the security of the complete processing of fuel.Therefore, be necessary from a large amount of refiltered oil products the separated trace removed
228th.Separation of Thorium and uranium the ore that in addition, also need to contain thorium and uranium from some.For the problems referred to above, in the urgent need to developing a kind of high efficiency Th-U separation and recovery method.
Ion exchange method is a kind of high efficiency separation method, and its equipment is simple, and operation is easily gone, and does not have be separated difficulty and solvent loss.Ion-exchanger has important position in the mask work of nuclear fuel recovery and fission product.Studying more is the isolation technique of inorganic ion exchanger and organic ion exchanger.But the former absorption property and the selectivity in strong acid medium is low, often need feed liquid to neutralize and denitration processing, make technical process complicated, and engineering efficiency is low, cost is high.The latter's acidproof, heat and irradiation stability are poor, therefore nuclear fuel reclaim and the separated practical application of fission product on be restricted.For these problems, there is investigator to propose to utilize the porous silica carrier of development, the Novel ion exchanger of making in the amino anionite-exchange resin load of aromatic series hand-hole is as main separation method, from analog fuel lysate and actual spent fuel lysate like a bomb Separation and Recovery U, Pu, Np and Tc, Ru(non-patent literature 1:Y.Z.Wei, T.Arai, H.Hoshi, M.Kumagai, A.Bruggeman, P.Goethals.Development of a New AqueousProcess for Nuclear Fuel Reprocessing:Hot Tests on the Recovery of U and Pu from a Nitric AcidSolution of Spent LWR fuel, Nuclear Technology, 149 (2005): 217-231.).Owing to ion exchange functional groups being loaded on silicon-dioxide base material, its chemical stability and radiation hardness stability have significantly been improved.At present, there is not yet under pertinent literature report high density nitric acid condition the report of separated Th and U.
Summary of the invention
The object of the present invention is to provide and a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery.
Goal of the invention of the present invention is achieved through the following technical solutions:
The object of the present invention is to provide and a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, comprising:
1) Pretreatment Engineering: the material dissolution that contains the radioelement such as thorium and uranium, in high density nitric acid, is formed to the nitrate solution of thorium and uranium;
2) absorption engineering: in above-mentioned nitric acid system, add anionite-exchange resin, carry out ion-exchange absorption;
3) drip washing engineering: after ion-exchange, adopt leacheate drip washing to be adsorbed on the thorium on anionite-exchange resin, can realize the Separation and Recovery of thorium and uranium.
Described high density concentration of nitric acid is 3-12mol/L; More excellent, the nitric acid of selection concentration 6-9mol/L, Separation and Recovery better effects if.
Described anionite-exchange resin is with SiO
2microballoon is carrier, is shaped as porousness spheroidal material, and mean diameter is 30-200 micron, mean pore size 10-500nm.
Described anionite-exchange resin is pyridines anionite-exchange resin.
Described pyridines anionite-exchange resin contains following functional group:
or
Described ion-exchange absorption can be carried out at ambient temperature.
Described leacheate is lower concentration aqueous nitric acid, and its concentration is lower than 1mol/L; More excellent, select the nitric acid of concentration below 0.01-0.1mol/L, drip washing separating effect is better.
The porous Si O that the present invention adopts
2microballoon is that the pyridines anionite-exchange resin of carrier is by situ polymerization method, to prepare to obtain (non-patent literature 2:Y-Z Wei; M Yamaguchi; M Kumagai; Y Takashima; T Hoshikawa; F Kawamura. " Separation of actinides from simulated spent fuel solutions by an advanced ion-exchange process " Journal of Alloys and Compounds.Volumes271 – 273; 12; 1998, Pages693-696; Non-patent literature 3:A.Zhang, Y.-Z.Wei, T.Arai and M.Kumagai, " Palladium Removal from the Simulated Nuclear Spent Fuel Solution Using a Silica-Based SiPyR-N3Anion Exchanger ", Solvent Extraction and Ion Exchange, 24,447-462 (2006)).Synthetic pyridines organic ion exchange composition is dispersed and is fixed in particle diameter 50-100 μ m porous support, the polymer exchanger of preparing from common chemical polymerization is different, because the polymkeric substance containing function base is limited in the macropore of silicon-dioxide, its adsorbing metal ions solution and the swelling that causes is restricted, so the pressure-losses producing when post is separated is very little.Anionite prepared by situ aggregation method is divided into: weak base anion-exchange resin (SiPyRN
3), strongly basic anion exchange resin (SiPyRN
4) and a kind of 4 grades, 3 grades of amine function groups respectively account for the composite anion exchange resin (AR-01) that has weakly alkaline and strong basicity dual-functional group concurrently of half.This class ion exchange resin, because ion-exchange group loads on silicon-dioxide base material, has improved acidproof, the heat-resisting and resistance to irradiation stability of exchanger.Following is that the contained chemical functional group structure of pyridines anionite-exchange resin is given an example.
By above-mentioned porous Si O
2microballoon is the Th dissolving in the pyridines anionite-exchange resin of carrier and high density nitric acid, the radioelement such as U contact and to carry out ion-exchange absorption attached, utilization is preferentially adsorbed Th to the absorption property difference of Th and U, when the radioelement such as Th are adsorbed on after above-mentioned anionite-exchange resin, further by leacheate, the thorium being adsorbed on anionite-exchange resin is carried out to drip washing, realize the Separation and Recovery of thorium and uranium.
Compared with prior art, beneficial effect of the present invention is as follows:
The present invention utilizes silica-based anionite-exchange resin to carry out Separation and Recovery to the thorium in the raw materials such as Nuclear Power Station's Exhausted Fuels (Th) and uranium (U) element, and this separation method is simple, and operation is easily gone, and does not have be separated difficulty and solvent loss, particularly porous SiO
2the use of carrier, has guaranteed its stability under peracid, strong irradiation application conditions.
Separation method of the present invention not only can be from the spent fuel of Th base nuclear fuel Separation and Recovery Th and U, also can reclaim the uranium product obtaining from light-water reactor uranium oxide spent fuel, the separated descendant Th-228 that removes U-232, has further ensured the security of industrial operation; Separation of Thorium and uranium in the ore that in addition, also can contain thorium and uranium at some.
The present invention is by utilizing Th and the U absorption property difference under different concns nitric acid environment, realized the Separation and Recovery of two kinds of elements, silica-based anionite-exchange resin used is leached rear reusable, not only effectively reduce cost, more can meet the industrial operational requirements to Dynamic adsorption, there is good industrial applications prospect.
Accompanying drawing explanation
Fig. 1 is 3 kinds of silica-based pyridines the anionite-exchange resin adsorption curve to Th and U, wherein a-SiPyRN under different concentration of nitric acid
3, b-SiPyRN
4, c-AR-01;
Fig. 2 is SiPyRN
4anionite-exchange resin carries out the solid phase chromatographic separation curve of fractionation by adsorption to Th/U blend solution;
Fig. 3 is SiPyRN
4anionite-exchange resin is to constant U, and the blend solution of micro-Th carries out the solid phase chromatographic separation curve of fractionation by adsorption.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
The Th that the present embodiment adsorption test is used and U solution are
238the nitrate of U and
232the nitrate mixed solution of Th, is the salpeter solution configuration 5ml of 0.5mol/L, 1mol/L, 3mol/L, 6mol/L, 9mol/L by concentration respectively, and Th and U ion starting point concentration are the nitrate mixed solution of 10mM, then under room temperature, drop into 0.1g SiO
2microballoon is the pyridines anionite-exchange resin SiPyRN of carrier
3carry out a batch adsorption test.
Above-mentioned adsorption test was at room temperature vibrated after 2 hours, reclaimed its supernatant liquor, thereby analyze its kish concentration with ICP light-dividing device, calculated it to Th and U absorption partition ratio (Kd).
Repeat aforesaid operations, select respectively SiO
2microballoon is the pyridines anionite-exchange resin SiPyRN of carrier
4, AR-01 substitutes SiPyRN
3carry out parallel laboratory test, result as shown in Figure 1, the SiPyRN that the present embodiment is used
3, SiPyRN
4and AR-01, its ion-exchange total amount is 3.2-4.4meq/g-resin.
By comparison diagram 1,3 kinds of pyridines anionite-exchange resin used in the present invention have good characterization of adsorption to Th under high acidity, and U is adsorbed hardly.This may be because U does not participate in the complexing of nitric acid in the higher nitric acid of concentration, so the very difficult nitric acid Anion-adsorption as complexing is on pyridines anionite-exchange resin.Thereby this shows can preferentially to adsorb in the salpeter solution of silica-based pyridines anionite-exchange resin used in the present invention more than 6M Th and realizes to a certain extent separated of Th and U.Particularly under the peracid condition of 6-9M nitric acid, more than the separation factor of Th and U (the absorption partition ratio of absorption partition ratio/U of Th equals the separation factor of the two, and separation is higher, and the two is more easily separated) can reach 5-10.Being adsorbed on Th on above-mentioned pyridines anionite-exchange resin can be by rare nitric acid (such as 0.1M nitric acid or pure water) Separation and Recovery after drip washing simply, and this separation and recovery method has very large actual application prospect.
Embodiment 2
The Th that the present embodiment adsorption test is used and U solution are
238the nitrate of U and
232the salpeter solution configuration 25ml that the nitrate mixed solution of Th is 9mol/L by concentration, Th and U ion starting point concentration are the nitrate mixed solution of 10mM.
Choose the SiPyRN stating in pyridines anionite-exchange resin
4resin is representative, and under moisture state, being filled into is highly 500mm, and diameter is 10mm, in the chromatographic separation post that volume is 39.25ml, with 9M salpeter solution, carries out pre-equilibration and confirms its dead volume (Dead Volume).
Pass into the Th that contains modulating in advance, the salpeter solution 25ml of U carries out Th, the stratography experiment of U fractionation by adsorption, the logical liquid speed of 25mlTh/U blend solution remains on 1ml/min and carries out dynamic adsorption, keep subsequently same flow velocity to pass into successively the 9M nitric acid of about 100ml and the 0.1M nitric acid leacheate of about 50ml and carry out separatedly, finally with the pure water of 100ml left and right, clean again.Dynamic adsorption experiment and the experiment of drip washing subsequently are all at room temperature carried out.Fig. 2 is for being used the SiPyRN in silica-based pyridines anionite-exchange resin
4th/U blend solution is carried out to the solid phase chromatographic separation experimental result of fractionation by adsorption.
Result by Fig. 2 can be seen, under 9M nitric acid system, utilizes silica-based pyridines anionite-exchange resin SiPyRN
4to Th, the different fractionation by adsorption effects of U element, absorption Th, the anionite-exchange resin of U is separated the first drip washing of the U in absorption in 9M nitric acid leacheate, and this time, Th still remained on anionite-exchange resin, and chromatography column liquid outlet can't detect Th.And at separation phase subsequently, change the nitric acid (0.1M nitric acid) that leacheate is used lower concentration, can very soon the Th on anionite-exchange resin be leached out.By aforesaid operations, can be by Th in whole system, U carries out thorough separation.
In embodiment 2, Th, the ratio of U in salpeter solution approaches, and utilizes pyridines anionite-exchange resin SiPyRN
4the difference of both adsorptive poweies is easy to carry out separation.Yet, in actual applications, often also can from some containing the solution of constant U, the Th that separated trace coexists.Such as reclaiming the uranium product obtaining from light-water reactor uranium oxide spent fuel, the separated descendant Th-228 that removes U-232.Under this condition, can Th/U completely separated, directly has influence on the application prospect of pyridines anionite-exchange resin.
Choose the SiPyRN stating in pyridines anionite-exchange resin
4resin is representative, under moisture state, being filled into is highly 100mm, and diameter is 10mm, in the chromatographic separation post that volume is 7.85ml, first with the 9M salpeter solution containing U of 10mM, with the logical liquid speed of 2ml/min, carry out dynamic saturated adsorption, until the outlet U concentration of chromatography column reaches 10mM.Use subsequently 10mM concentration as the concentration of constant U, in 9M nitric acid, chromatography column carried out to pre-equilibration and confirm its dead volume (Dead Volume).
The Th that the present embodiment adsorption test is used and U solution are
238the nitrate of U and
232the salpeter solution configuration 25ml nitrate mixed solution that the nitrate mixed solution of Th is 9mol/L by concentration, the starting point concentration of constant U is 10mM, the starting point concentration of micro-Th is modulated to 0.1mM.
Pass into the micro-Th that contains modulating in advance, the salpeter solution 25ml of constant U carries out Th, the stratography experiment of U fractionation by adsorption, the logical liquid speed of 25mlTh/U blend solution remains on 2ml/min and carries out dynamic adsorption, keep subsequently same flow velocity to pass into successively the 9M nitric acid of about 100ml and the 0.1M nitric acid leacheate of about 50ml and carry out separatedly, finally with the pure water of 100ml left and right, clean again.All adsorption experiments and the experiment of drip washing subsequently are all at room temperature carried out.Fig. 3 is for being used the SiPyRN in silica-based pyridines anionite-exchange resin
4to constant U, the blend solution of micro-Th carries out the solid phase chromatographic separation experimental result of fractionation by adsorption.
Result by Fig. 3 can be seen, under 9M nitric acid system, utilizes silica-based pyridines anionite-exchange resin SiPyRN
4to Th, the different fractionation by adsorption effects of U element, even polymeric adsorbent saturated adsorption U in advance, also can the U of micro-Th and constant is thoroughly separated in experiment subsequently.Even if be adsorbed onto micro-Th on chromatography column under 100 times of concentration U exist, still can be preferentially adsorbed on the anionite-exchange resin of saturated adsorption U, and at separation phase subsequently, change the nitric acid (0.1M nitric acid) that leacheate is used lower concentration, can very soon the Th on anionite-exchange resin be leached out.By aforesaid operations, can be by micro-Th in whole system, constant U carries out thorough separation.
Although the present invention discloses preferred embodiment as above; so it is not in order to limit content of the present invention; anyly be familiar with this skill person; within not departing from main spirits of the present invention and context; when doing various changes and retouching, therefore the protection domain of invention should be as the criterion with the basic right claimed range of applying for a patent.
Claims (8)
1. utilize silica-based anionite-exchange resin thorium and uranium to be carried out to a method for Separation and Recovery, comprising:
1) Pretreatment Engineering: the material dissolution that contains the radioelement such as thorium and uranium, in high density nitric acid, is formed to the nitrate solution of thorium and uranium;
2) absorption engineering: in above-mentioned nitric acid system, add anionite-exchange resin, carry out ion-exchange absorption;
3) drip washing engineering: after ion-exchange, adopt leacheate drip washing to be adsorbed on the thorium on anionite-exchange resin, can realize the Separation and Recovery of thorium and uranium.
2. according to claim 1ly a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, it is characterized in that: described high density concentration of nitric acid is 3-12mol/L.
3. according to claim 2ly a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, it is characterized in that: described high density concentration of nitric acid is 6-9mol/L.
4. according to claim 1ly a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, it is characterized in that: described anionite-exchange resin is with SiO
2microballoon is carrier, is shaped as porousness spheroidal material, and mean diameter is 30-200 micron, mean pore size 10-500nm.
5. according to claim 4ly a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, it is characterized in that: described anionite-exchange resin is pyridines anionite-exchange resin.
6. according to claim 5ly a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, it is characterized in that: described pyridines anionite-exchange resin contains following functional group:
or
7. according to claim 1ly a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, it is characterized in that: described leacheate is lower concentration aqueous nitric acid, and its concentration is lower than 1mol/L.
8. according to claim 7ly a kind ofly utilize silica-based anionite-exchange resin thorium and uranium to be carried out to the method for Separation and Recovery, it is characterized in that: described leacheate is that concentration is at the nitric acid of 0.01-0.1mol/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498739A (en) * | 2014-12-02 | 2015-04-08 | 益阳鸿源稀土有限责任公司 | Method for separating and recycling uranium, thorium and rare earth in rare earth mineral decomposition residue |
| CN105425274A (en) * | 2015-12-02 | 2016-03-23 | 中国原子能科学研究院 | Measurement and determination method for age of uranium sample |
| CN107004450A (en) * | 2014-11-19 | 2017-08-01 | 阿海珐有限公司 | Method and apparatus for reclaiming radionuclide from the resin material after |
| CN108396146A (en) * | 2018-03-01 | 2018-08-14 | 常熟理工学院 | The adsorption treatment method and device of thorium element in rare earth waste |
| CN111269339A (en) * | 2020-01-21 | 2020-06-12 | 广西大学 | Silicon-based anion exchange resin and preparation method thereof |
| CN111426764A (en) * | 2020-04-09 | 2020-07-17 | 中国科学院地质与地球物理研究所 | Method for testing age of hydrothermal sulfide in quaternary seabed |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107004450A (en) * | 2014-11-19 | 2017-08-01 | 阿海珐有限公司 | Method and apparatus for reclaiming radionuclide from the resin material after |
| CN107004450B (en) * | 2014-11-19 | 2019-05-21 | 法玛通有限公司 | Method and apparatus for recycling radionuclide from the resin material after |
| CN104498739A (en) * | 2014-12-02 | 2015-04-08 | 益阳鸿源稀土有限责任公司 | Method for separating and recycling uranium, thorium and rare earth in rare earth mineral decomposition residue |
| CN104498739B (en) * | 2014-12-02 | 2016-03-09 | 益阳鸿源稀土有限责任公司 | A kind of rare-earth mineral decomposes the separation and recovery method of uranium, thorium, rare earth in recrement |
| CN105425274A (en) * | 2015-12-02 | 2016-03-23 | 中国原子能科学研究院 | Measurement and determination method for age of uranium sample |
| CN108396146A (en) * | 2018-03-01 | 2018-08-14 | 常熟理工学院 | The adsorption treatment method and device of thorium element in rare earth waste |
| CN111269339A (en) * | 2020-01-21 | 2020-06-12 | 广西大学 | Silicon-based anion exchange resin and preparation method thereof |
| CN111426764A (en) * | 2020-04-09 | 2020-07-17 | 中国科学院地质与地球物理研究所 | Method for testing age of hydrothermal sulfide in quaternary seabed |
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