CN103589866B - 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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- CN103589866B CN103589866B CN201310627541.2A CN201310627541A CN103589866B CN 103589866 B CN103589866 B CN 103589866B CN 201310627541 A CN201310627541 A CN 201310627541A CN 103589866 B CN103589866 B CN 103589866B
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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 to carry out the method for Separation and Recovery to thorium and uranium.
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, and in order to utilize thorium in nuclear energy engineering, needing will by a series of nuclear reaction
232th is transformed into fissile material
233u.This series of nuclear reaction is carried out in reactor, easy 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, just defines Th-U Fuel cycle.The object elements needing 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, Th-U separation and recovery method many places are in conceptual phase, also do not occur efficient recovery method at present.In addition, reclaim the uranium product obtained from light-water reactor uranium oxide spent fuel, containing trace (0.5 ~ 4ppb/U)
23272 years U(transformation period), its descendant
2281.9 years Th(transformation period) through the multistage further descendant generated that decays
21260.6 minutes Bi(transformation period) and
2083 minutes Ti(transformation period) high-octane gamma-rays can be released, have a strong impact on and reclaim the security of uranium as the complete processing of fuel.Therefore, be necessary from a large amount of refiltered oil products be separated remove trace
228th.In addition, also need to contain Separation of Thorium and uranium the ore of 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, operates easy, there is not be separated difficulty and solvent loss.Ion-exchanger nuclear fuel reclaim and fission product mask work in have important position.Studying more is the isolation technique of inorganic ion exchanger and organic ion exchanger.But the former absorption property in strong acid medium and selectivity low, often need to neutralize feed liquid and denitration process, make technical process complicated, and engineering efficiency is low, cost is high.Acidproof, the hot and irradiation stability of the latter is poor, is therefore restricted in nuclear fuel recovery with the practical application be separated of fission product.For these problems, investigator is had to propose to utilize the porous silica carrier of development, using the Novel ion exchanger made in amino for aromatic series anionite-exchange resin load hand-hole as main sorting method, Separation and Recovery U like a bomb from the spent fuel lysate of analog fuel lysate and reality, 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 onthe Recovery of U and Pu from a Nitric AcidSolution of Spent LWR fuel, NuclearTechnology, 149 (2005): 217-231.).Owing to ion exchange functional groups being loaded on silicon-dioxide base material, significantly improve its chemical stability and radiation hardness stability.At present, under there is not yet pertinent literature report high density nitric acid condition, the report of Th and U is separated.
Summary of the invention
The object of the present invention is to provide and a kind ofly utilize silica-based anionite-exchange resin to carry out the method for Separation and Recovery to thorium and uranium.
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 to carry out the method for Separation and Recovery to thorium and uranium, comprising:
1) Pretreatment Engineering: by the material dissolution containing the radioelement such as thorium and uranium in high density nitric acid, forms the nitrate solution of thorium and uranium;
2) engineering is adsorbed: in above-mentioned nitric acid system, add anionite-exchange resin, carry out ion-exchange absorption;
3) drip washing engineering: after ion-exchange, the drip washing of employing leacheate is 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, select the nitric acid of concentration 6-9mol/L, Separation and Recovery better effects if.
Described anionite-exchange resin is with SiO
2microballoon is carrier, and shape is 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 is containing, for example lower 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 concentration at the nitric acid of below 0.01-0.1mol/L, drip washing separating effect is better.
The porous Si O that the present invention adopts
2microballoon is the pyridines anionite-exchange resin of carrier is prepared by situ polymerization method 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 advancedion-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, " PalladiumRemoval from the Simulated Nuclear Spent Fuel Solution Using a Silica-Based SiPyR-N3AnionExchanger ", Solvent Extraction and Ion Exchange, 24,447-462 (2006)).The pyridines organic ion of synthesis exchanges composition and is dispersed and fixed in particle diameter 50-100 μm porous support, different from polymer exchanger prepared by common chemical polymerization, because the polymkeric substance containing function base is limited in the macropore of silicon-dioxide, its adsorbing metal ions solution and being swellingly restricted of causing, so the pressure-losses produced 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) having weakly alkaline and strong basicity dual-functional group concurrently of half.This kind of ion exchange resin loads on silicon-dioxide base material due to ion-exchange group, improves acidproof, the heat-resisting and resistance to irradiation stability of exchanger.Following is chemical functional group structure example contained by pyridines anionite-exchange resin.
By above-mentioned porous Si O
2microballoon is the Th dissolved in the pyridines anionite-exchange resin of carrier and high density nitric acid, the radioelement such as U carry out contacting and to carry out ion-exchange absorption attached, utilize the absorption property difference Preferential adsorption Th to Th and U, after the radioelement such as Th are adsorbed on above-mentioned anionite-exchange resin, further by leacheate, drip washing is carried out to the thorium be adsorbed on anionite-exchange resin, 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 (Th) in the raw materials such as Nuclear Power Station's Exhausted Fuels and uranium (U) element, and this separation method is simple, operates easy, there is not be separated difficulty and solvent loss, particularly porous SiO
2the use of carrier, ensure that its stability under peracid, strong irradiation application conditions.
Separation method of the present invention not only can from the spent fuel of Th base nuclear fuel Separation and Recovery Th and U, also can reclaim the uranium product obtained from light-water reactor uranium oxide spent fuel, be separated the descendant Th-228 removing U-232, ensure the security of industrial operation further; In addition, Separation of Thorium and uranium in the ore that also can contain thorium and uranium at some.
The present invention is by utilizing the absorption property difference of Th and U under different concns nitric acid environment, achieve 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 be 3 kinds of silica-based pyridines anionite-exchange resin under different concentration of nitric acid to the adsorption curve of Th and U, wherein a-SiPyRN
3, b-SiPyRN
4, c-AR-01;
Fig. 2 is SiPyRN
4anionite-exchange resin carries out the solid phase chromatography detach Spline 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 chromatography detach Spline of fractionation by adsorption.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
The present embodiment adsorption test Th and U solution used is
238the nitrate of U and
232the nitrate mixed solution of Th, is the nitrate mixed solution of 10mM respectively, then under room temperature, drops into 0.1g SiO with salpeter solution configuration 5ml, Th and the U ion starting point concentration that concentration is 0.5mol/L, 1mol/L, 3mol/L, 6mol/L, 9mol/L
2microballoon is the pyridines anionite-exchange resin SiPyRN of carrier
3carry out a batch adsorption test.
After above-mentioned adsorption test is at room temperature vibrated 2 hours, reclaim its supernatant liquor, analyze its kish concentration with ICP light-dividing device thus calculate it to Th and U adsorption isothermequation (Kd).
Repeat aforesaid operations, select SiO respectively
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 highly acidity, and U is then adsorbed hardly.This may be because U does not participate in the complexing of nitric acid in the nitric acid that concentration is higher, so the nitric acid anions be difficult to as complexing is adsorbed on pyridines anionite-exchange resin.This shows that silica-based pyridines anionite-exchange resin used in the present invention can Preferential adsorption Th thus realize Th with U being separated to a certain extent in the salpeter solution of more than 6M.Particularly under the peracid condition of 6-9M nitric acid, the separation factor (adsorption isothermequation of the adsorption isothermequation/U of Th equals the separation factor between the two, and be separated higher, the two is more easily separated) of Th and U can reach more than 5-10.The Th be adsorbed on above-mentioned pyridines anionite-exchange resin can use dust technology (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 present embodiment adsorption test Th and U solution used is
238the nitrate of U and
232the nitrate mixed solution of Th, is the nitrate mixed solution of 10mM with salpeter solution configuration 25ml, Th and the U ion starting point concentration that concentration is 9mol/L.
Choose the SiPyRN stated in pyridines anionite-exchange resin
4resin is representative, and being filled under moisture state is highly 500mm, and diameter is 10mm, and volume is in the chromatographic separation post of 39.25ml, carries out pre-equilibration and confirm its dead volume (Dead Volume) with 9M salpeter solution.
Pass into modulate in advance containing Th, the salpeter solution 25ml of U carries out Th, the stratography experiment of U fractionation by adsorption, 25mlTh/U blend solution leads to liquid speed and remains on 1ml/min and carry out dynamic adsorption, the 0.1M nitric acid leacheate of the 9M nitric acid and about 50ml that keep same flow velocity to pass into about 100ml successively is subsequently separated, and finally cleans with the pure water of about 100ml again.Dynamic adsorption experiment and the experiment of drip washing subsequently are all at room temperature carried out.Fig. 2 uses the SiPyRN in silica-based pyridines anionite-exchange resin
4th/U blend solution is carried out to the solid phase chromatography separating experiment result of fractionation by adsorption.
Can be seen by the result of Fig. 2, under 9M nitric acid system, utilize silica-based pyridines anionite-exchange resin SiPyRN
4to the different fractionation by adsorption effects of Th, U element, first for the U in absorption drip washing is separated by the anionite-exchange resin of absorption Th, U 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 uses lower concentration, can very fast Th on anionite-exchange resin be leached out.By aforesaid operations, Th, U in whole system thoroughly can be separated.
Embodiment 3
In embodiment 2, Th, the U ratio in salpeter solution is close, utilizes pyridines anionite-exchange resin SiPyRN
4be easy to be separated to the difference of both adsorptive poweies.But, in actual applications, often also can need from some containing the solution of constant U, be separated the Th that coexists of trace.Such as reclaim the uranium product obtained from light-water reactor uranium oxide spent fuel, be separated the descendant Th-228 removing U-232.Under these conditions, can Th/U be separated completely, directly has influence on the application prospect of pyridines anionite-exchange resin.
Choose the SiPyRN stated in pyridines anionite-exchange resin
4resin is representative, being filled under moisture state is highly 100mm, and diameter is 10mm, and volume is in the chromatographic separation post of 7.85ml, first lead to liquid speed with the 9M salpeter solution containing U of 10mM with 2ml/min and carry out dynamic saturated adsorption, until the outlet U concentration of chromatography column reaches 10mM.Use 10mM concentration as the concentration of constant U subsequently, in 9M nitric acid, pre-equilibration carried out to chromatography column and confirm its dead volume (DeadVolume).
The present embodiment adsorption test Th and U solution used is
238the nitrate of U and
232the nitrate mixed solution of Th, be the salpeter solution configuration 25ml nitrate mixed solution of 9mol/L by concentration, the starting point concentration of constant U is 10mM, and the starting point concentration of micro-Th is modulated to 0.1mM.
Pass into modulate in advance containing micro-Th, the salpeter solution 25ml of constant U carries out Th, the stratography experiment of U fractionation by adsorption, 25mlTh/U blend solution leads to liquid speed and remains on 2ml/min and carry out dynamic adsorption, the 0.1M nitric acid leacheate of the 9M nitric acid and about 50ml that keep same flow velocity to pass into about 100ml successively is subsequently separated, and finally cleans with the pure water of about 100ml again.All adsorption experiments and the experiment of drip washing subsequently are all at room temperature carried out.Fig. 3 uses the SiPyRN in silica-based pyridines anionite-exchange resin
4to constant U, the blend solution of micro-Th carries out the solid phase chromatography separating experiment result of fractionation by adsorption.
Can be seen by the result of Fig. 3, under 9M nitric acid system, utilize silica-based pyridines anionite-exchange resin SiPyRN
4to the different fractionation by adsorption effects of Th, U element, even if polymeric adsorbent saturated adsorption U in advance, also the Th of trace thoroughly can be separated with the U of constant in experiment subsequently.Even if the micro-Th be adsorbed onto on chromatography column is 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 uses lower concentration, can very fast Th on anionite-exchange resin be leached out.By aforesaid operations, can by Th micro-in whole system, constant U is thoroughly separated.
Although preferred embodiment discloses as above by the present invention; so itself and be not used to limit content of the present invention; anyly be familiar with this those skilled in the art; not departing from main spirits of the present invention and context; when doing various change and retouching, the protection domain therefore invented should be as the criterion with the basic right claimed range applied for a patent.
Claims (5)
1. utilize silica-based anionite-exchange resin to carry out a method for Separation and Recovery to thorium and uranium, comprising:
1) Pretreatment Engineering: the high density nitric acid by the material dissolution containing thorium and uranium radioelement in concentration being 3-12mol/L, forms the nitrate solution of thorium and uranium;
2) engineering is adsorbed: in above-mentioned nitric acid system, add anionite-exchange resin, carry out ion-exchange absorption, described anionite-exchange resin is the pyridines anionite-exchange resin containing, for example lower functional group:
3) drip washing engineering: after ion-exchange, the drip washing of employing leacheate is 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 to carry out the method for Separation and Recovery to thorium and uranium, it is characterized in that: described high density concentration of nitric acid is 6-9mol/L.
3. according to claim 1ly a kind ofly utilize silica-based anionite-exchange resin to carry out the method for Separation and Recovery to thorium and uranium, it is characterized in that: described anionite-exchange resin is with SiO
2microballoon is carrier, and shape is porousness spheroidal material, and mean diameter is 30-200 micron, mean pore size 10-500nm.
4. according to claim 1ly a kind ofly utilize silica-based anionite-exchange resin to carry out the method for Separation and Recovery to thorium and uranium, it is characterized in that: described leacheate is lower concentration aqueous nitric acid, and its concentration is lower than 1mol/L.
5. according to claim 4ly a kind ofly utilize silica-based anionite-exchange resin to carry out the method for Separation and Recovery to thorium and uranium, it is characterized in that: described leacheate is the nitric acid of concentration at 0.01-0.1mol/L.
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| EP3221048B1 (en) * | 2014-11-19 | 2018-10-10 | Framatome GmbH | Method and apparatus for the recovery of radioactive nuclides from spent resin materials |
| 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 |
| CN111426764B (en) * | 2020-04-09 | 2020-10-27 | 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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| CN103014359A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Separation and recovery method of monazite slag |
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| US2943923A (en) * | 1958-02-10 | 1960-07-05 | Ca Atomic Energy Ltd | Processing of nitrate solutions containing thorium and uranium 233 |
| CN103014359A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Separation and recovery method of monazite slag |
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