CN103409649A - Method and device for reducing, extracting and separating rear earth through fused salt and liquid metal - Google Patents
Method and device for reducing, extracting and separating rear earth through fused salt and liquid metal Download PDFInfo
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- CN103409649A CN103409649A CN2013102197560A CN201310219756A CN103409649A CN 103409649 A CN103409649 A CN 103409649A CN 2013102197560 A CN2013102197560 A CN 2013102197560A CN 201310219756 A CN201310219756 A CN 201310219756A CN 103409649 A CN103409649 A CN 103409649A
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Abstract
The invention provides a method and a device for reducing, extracting and separating rear earth through fused salt and liquid metal. Liquid aluminum serves as a cathode, a graphite rod serves as an anode, KCl-LiCl is added into an electrolytic cell to be heated and smelted to serve as electrolyte, and lithium obtained from electrolysis at the cathode is dissolved in the liquid aluminum to obtain a liquid aluminum-lithium alloy by means of electrolysis; praseodymium chloride and samarium chloride are added into the electrolytic cell to serve as a fused salt phase, and a constant speed stirring extraction reaction is carried out in an argon atmosphere with the liquid aluminum-lithium alloy as an extraction agent; the fused salt phase is separated from a liquid metal phase, samarium is extracted into the liquid metal phase to form an aluminum-lithium-samarium alloy, and praseodymium is left in the fused salt phase so as to separate the samarium from the praseodymium. The method and the device provided by the invention are suitable for extreme conditions such as high temperature, and strong radiation; the reducing agent can be recycled to save resources; the distribution coefficient of the samarium in the alloy and the fused salt is 68.1-142.4, the distribution coefficient of the praseodymium in the alloy and the fused salt is 2.9-23.2, and the samarium-praseodymium separation coefficient is 5.0-23.3.
Description
Technical field
What the present invention relates to is a kind of separation method of rare earth.Page of the present invention relates to a kind of tripping device of rare earth.
Background technology
Develop actively nuclear energy, can alleviate not only that China is near, the pressure of power supply in mid-term anxiety, and long-term stability supply and even the Sustainable Socioeconomic Development of China's energy had to extremely important strategic importance.At present, China's nuclear power developing paces are obviously accelerated, and expect the installed capacity of the year two thousand twenty nuclear power and are expected near 80GW.Measuring and calculating accordingly, the storage capacity of China's Nuclear Power Station's Exhausted Fuels accumulation when the time comes will be over 10000 tons, and the annual spent fuel drawn off from Nuclear power plants is near 1700 tons.From the angle that uranium resources effectively utilizes and nuclear environment is protected, spent fuel is carried out to aftertreatment significant.
The spent fuel post-processing technology can be divided into water law aftertreatment and two kinds of technology of dry method (mainly referring to molten-salt growth method) aftertreatment according to the medium used.The dry method post-processing technology is applicable to thermal reactor spent fuel and the aftertreatment of fast reactor spent fuel fuel that cooling time is short, burnup is dark, is the spent fuel post-processing technology with development potentiality.Rare earth element in spent fuel is close with actinide elements character, and many rare earth elements are again neutron poisons, therefore will realize the part recycle of spent fuel, the rare earths separation in spent fuel must be gone out.
The basic skills of rare earths separation has: step-by-step precipitation method, fractionation crystallization, solvent extration, ion exchange method and chemical gas phase transmission etc.At present solvent extration has now become the main method of domestic and international Rare Earth Separation, and research and the process optimization of its extraction mechanisms is subject to people's attention day by day.For example number of patent application is 200710098732.9, name is called in the patent document of " from the processing method of extraction separation of quadravalence cerium, thorium, fluorine and few cerium trivalent rare earth rare earth sulfate solution ", disclose a kind of employing and carried out extracting and separating based on the synergic reagent of P507 or P204, cerium (IV), thorium, fluorine, iron are extracted into organic phase, then the proceed step by step selectivity is washed and back extraction, obtains the method for cerium oxide, Thorotrast, fluorine chemical product.Yet spent fuel or target spare have the characteristics of high burnup, high irradiation, this makes traditional water law aftertreatment flow process be difficult to meet the separation needs.In the process of dry method aftertreatment (dry reprocessing), do not make water as solvent, its main separating step at high temperature carries out.Flow process has the advantages such as anti-irradiation, low critical risk, radwaste are few, suitable treatment high burnup, short cooling stage spent fuel.Fused salt/the liquid metal of take has bright application prospect in spent fuel aftertreatment field as the dry method post-processing technology of medium.For example patent publication No. is CN202155172U, name is called in the patent document of " fused-salt extraction stirring paddle device ", reported that openly the fused salt extraction whipping appts mainly is applicable to the test production of radioactivity material, the fields such as abstraction purification, be applied to the mixing of material in its pyrochemistry process, contact, extraction, the aspects such as chemical reaction, for the mixing of applying between the material in the pyrochemistry system, reaction etc. provides dynamical foundation and fluid basis, make the mixing of pyrochemistry process implementation material, contact and then reach the extraction between material, separation and purification and (or) purpose such as chemical reaction, also may extend to application in other pyrochemistry tests and production.
The present invention is to provide the method for a kind of fused salt/liquid metal reduction extraction rare-earth separating.Article " Distribution behavior of uranium according to people such as M.Kurata, neptunium, rare-earth elements (Y, La, Ce, Nd, Sm, Eu, Gd) and alkaline-earth metals (Sr, Ba) between molten LiCl-KCI eutectic salt and liquid cadmium or bismuth, Journal of Nuclear Materials, 227, 110-121P " middle calculation of distribution coefficient (formula 1, 2) and the method for separation factor (formula 3) calculate Sm and partition ratio and the separation factor of Pr in alloy and fused salt.
β
1=D
Sm/D
Pr (3)
Wherein: D
Sm, D
PrFor Sm, Pr partition ratio;
Be respectively Sm, the Pr molar fraction in alloy and fused salt, β
1Separation factor for samarium and Pr.
Summary of the invention
The object of the present invention is to provide a kind of process simple, can be under the extreme conditions such as high temperature, severe radiation the effectively fused salt of extracting rare-earth element and the method for liquid metal reduction extraction rare-earth separating.The present invention also aims to provide the device of a kind of fused salt and liquid metal reduction extraction rare-earth separating.
The object of the present invention is achieved like this:
The method of fused salt of the present invention and liquid metal reduction extraction rare-earth separating comprises the steps:
A, prepare reductive agent: the employing liquid aluminium is negative electrode, anode adopts the spectroscopically pure graphite rod, and massfraction is joined in electrolyzer after heat fused as ionogen, under 750-900 ℃ than the KCl-LiCl mixture that is 50～54%:40～44%, carry out electrolysis, cathode current density is 1.3Acm
-2, bath voltage is 4-5.4V, and through electrolysis in 240-300 minute, catholyte gained lithium was dissolved in liquid aluminium, and obtaining lithium content is 3%-6wt% liquid aluminium lithium alloy liquid aluminium lithium alloy;
B, extractive reaction: take out anode and negative electrode conductive filament, to add in electrolyzer account for ionogen 0.5%-1.6wt% praseodymium chloride with the samarium trichloride mixed chlorinated rare earth as the fused salt phase, the liquid aluminium lithium alloy of gained of usining mixes it with fused salt mutually as liquid metal, the fused salt phase is 29-35:1 with the volume ratio of liquid metal phase, and the liquid aluminium lithium alloy of take at the uniform velocity stirs 3-7 hour extractive reaction as extraction agent under argon gas atmosphere protection;
C, separation: question response fully after, stop stirring, standing 0.5-1 hour, open purging valve, separates fused salt phase and liquid metal phase, samarium be extracted to liquid metal mutually in and form aluminum-lithium-samarium alloy, praseodymium stay fused salt mutually in, samarium is separated with praseodymium.The partition ratio of samarium in alloy and fused salt is 68.1-142.4, and the partition ratio of praseodymium in alloy and fused salt is 2.9-23.2, and samarium praseodymium separation factor is 5.0-23.3.
The method of fused salt of the present invention and liquid metal reduction extraction rare-earth separating can also comprise:
1, the fused salt phase recycle after the separation.
2, the described stir speed (S.S.) at the uniform velocity stirred is 60-240 rev/min.
3, described LiCl and KCl are respectively 300 ℃, 600 ℃ drying treatment 24 hours.
The device of fused salt of the present invention and liquid metal reduction extraction rare-earth separating comprises electrolyzer 3, thermopair 2, anode 1, negative electrode, electrolyzer is placed in pit furnace, KCl-LiCl fused salt 4 is housed in electrolyzer, described anode is graphite rod, described negative electrode comprises crucible 6, is loaded on liquid aluminium 5 and molybdenum filament 7 in crucible, the molybdenum filament overcoat has the silica tube bottom to be dipped in liquid aluminium, draws together crucible, anode lower end and thermopair lower end and is dipped in fused salt, and inflation valve 9 and purging valve 10 are set on pit furnace.
What the present invention adopted is that the electrolysis fused salt prepares the simple substance lithium, displacement reduction, the method for liquid metal aluminium extracting and separating rear earth praseodymium, samarium.Principle of the present invention is that Constant Electric Current solves the simple substance lithium on liquid cathode aluminium, adds praseodymium chloride and samarium trichloride, carries out following reaction: the 3Li(alloy)+Pr
3+(fused salt) → 3Li
+(fused salt)+Pr(alloy), 3Li(alloy)+Sm
3+(fused salt) → 3Li
+(fused salt)+Sm(alloy), reduction of rare earth, according to praseodymium, the samarium ion difference of solubleness in electronegativity and liquid aluminium in eutectic LiCl-KCl system, finally reach the purpose of rare-earth separating.
Characteristics of the present invention are: (1) adopts fused salt/liquid metal system, with respect to the organic solvent of liquid extraction, is applicable to the extreme conditions such as high temperature severe radiation; (2) reductive agent by fused salt electrolysis system, can recycle, and economizes on resources; (3) volume of material of high-temperature molten salt extraction is little, is conducive to device miniaturization; (4) the Sm element is the changeable valence rare earth element, and in fused salt, its metal ion not exclusively discharges, and is difficult to become metal in cathodic reduction, and the electrolytic preparation changeable valence rare earth is the difficult problem in electrolysis field always.The present invention adopts the method for reduction extraction, and the partition ratio of samarium in alloy and fused salt is 68.1-142.4, and the partition ratio of praseodymium in alloy and fused salt is 2.9-23.2, and samarium praseodymium separation factor is 5.0-23.3.
The accompanying drawing explanation
Fig. 1 is the structural representation of the method equipment therefor of fused salt of the present invention and liquid metal reduction extraction rare earth.
Embodiment
In conjunction with Fig. 1; the device of fused salt of the present invention and liquid metal reduction extraction rare-earth separating comprises: 1, anode (spectroscopically pure graphite rod), 2, thermopair, 3, corundum crucible; 4, fused salt (eutectic KCl-LiCl); 5, liquid aluminium, 6, monkey, 7, molybdenum filament; 5,6,7 form negative electrode; 8 shielding gas (argon gas), 9, inflation valve, 10, purging valve.Concrete operation step: the device that fused salt electrolysis prepares reductive agent as shown in drawings, after making the liquid aluminium lithium alloy, while carrying out extractive reaction, take off electrode 1 and 7, liquid aluminium lithium alloy 5 is poured in fused salt, takes out monkey 6, loads onto the molybdenum stirring rake, open inflation valve 9 and be filled with argon gas, inflation rate 3-5L/min.After extractive reaction completes, stop stirring, standing 0.5-1 hour, open purging valve 10, separates fused salt phase and metallographic phase.
Below for example the method for fused salt of the present invention and liquid metal reduction extraction rare-earth separating is described in more detail:
Embodiment 1, a, reductive agent preparation: negative electrode adopts liquid aluminium, anode adopts the spectroscopically pure graphite rod, to hang down eutectic KCl-LiCl(massfraction than for 51:43%) mixture joins in electrolyzer after heat fused as ionogen, under 800 ℃, carry out constant-current electrolysis, cathode current density is 1.3Acm
-2, bath voltage 4.0-5.5V.Through electrolysis in 300 minutes, cathodic electricity solved lithium, was dissolved in liquid aluminium 4.8wt%, made the liquid aluminium lithium alloy; B, extractive reaction: take out anode and molybdenum filament, the liquid aluminium lithium alloy of gained of take is extraction agent, adds the PrCl of 0.6wt%
3, the SmCl of 0.6wt%
3, containing fused salt and the liquid metal phase volume ratio of mixing rare earth chloride is 29:1.Open inflation valve, be filled with argon gas, inflation rate 5L/min, under the argon gas atmosphere protection, 60 rev/mins were stirred 7 hours; C, separation: after question response is complete, stop stirring, standing 1 hour, open purging valve, pour out fused salt, obtain aluminum-lithium-samarium alloy 7.1g.Al in alloy, Li, Pr, Sm content are recorded by ICP, and content is than being 93.1%:2.2%:0.3%:4.4%, and 68.1% samarium is extracted in metallographic phase, and partition ratio is 68.1; 91.5% praseodymium is stayed in salt, and partition ratio is 2.9, and the separation factor of samarium praseodymium is 23.3.
Embodiment 2:a, reductive agent preparation: negative electrode adopts liquid aluminium, anode adopts the spectroscopically pure graphite rod, to hang down eutectic KCl-LiCl(massfraction than for 51:43%) mixture joins in electrolyzer after heat fused as ionogen, under 900 ℃, carry out constant-current electrolysis, cathode current density is 1.3Acm
-2, bath voltage 4.0-5.5V.Through electrolysis in 240 minutes, cathodic electricity solved lithium, was dissolved in liquid aluminium 3.7wt%, made the liquid aluminium lithium alloy; B, extractive reaction: take out anode and molybdenum filament, the liquid aluminium lithium alloy of gained of take is extraction agent, adds the PrCl of 1.5wt%
3, the SmCl of 0.8wt%
3, containing fused salt and the liquid metal phase volume ratio of mixing rare earth chloride is 35:1.Open inflation valve, be filled with argon gas, inflation rate 3L/min, under the argon gas atmosphere protection, 240 rev/mins were stirred 3 hours; C, separation: after question response is complete, stop stirring, standing 0.5 hour, open purging valve, pour out fused salt, obtain aluminum-lithium-samarium alloy 3.7g.Al in alloy, Li, Pr, Sm content are recorded by ICP, and content is than being 84.5%:10.1%:0.9%:4.5%, and 61.8% samarium is extracted in metallographic phase, and partition ratio is 115.8; 94% praseodymium is stayed in salt, and partition ratio is 23.2, and the separation factor of samarium praseodymium is 5.0.
Embodiment 3:a, reductive agent preparation: negative electrode adopts liquid aluminium, anode adopts the spectroscopically pure graphite rod, to hang down eutectic KCl-LiCl(massfraction than for 50.5:43%) mixture joins in electrolyzer after heat fused as ionogen, under 900 ℃, carry out constant-current electrolysis, cathode current density is 1.3Acm
-2, bath voltage 4.0-5.5V.Through electrolysis in 300 minutes, cathodic electricity solved lithium, was dissolved in liquid aluminium 4.5wt%, made the liquid aluminium lithium alloy; B, extractive reaction: take out anode and molybdenum filament, the liquid aluminium lithium alloy of gained of take is extraction agent, adds the PrCl of 0.8wt%
3, the SmCl of 1.2wt%
3, containing fused salt and the liquid metal phase volume ratio of mixing rare earth chloride is 29:1.Open inflation valve, be filled with argon gas, inflation rate 5L/min, under the argon gas atmosphere protection, 240 rev/mins were stirred 3 hours; C, separation: after question response is complete, stop stirring, standing 0.5 hour, open purging valve, pour out fused salt, obtain aluminum-lithium-samarium alloy 4.1g.Al in alloy, Li, Pr, Sm content are recorded by ICP, and content is than being 88.2%:2.0%:1.6%:8.2%, and 82.4% samarium is extracted in metallographic phase, partition ratio is 142.3,31.1% praseodymium is stayed in salt, and partition ratio is 13.4, and the separation factor of samarium praseodymium is 10.5.
Claims (6)
1. the method for a fused salt and liquid metal reduction extraction rare-earth separating, is characterized in that comprising the steps:
A, prepare reductive agent: adopting the 3%-6wt% liquid aluminium is negative electrode, anode adopts graphite rod, and massfraction is joined in electrolyzer after heat fused as ionogen, under 750-900 ℃ than the KCl-LiCl mixture that is 50～54%:40～44%, carry out electrolysis, cathode current density is 1.3Acm
-2, bath voltage is 4-5.4V, and through electrolysis in 240-300 minute, catholyte gained lithium was dissolved in liquid aluminium, and obtaining lithium content is 3%-6wt% liquid aluminium lithium alloy;
B, extractive reaction: take out anode and negative electrode conductive filament, to add in electrolyzer account for ionogen 0.5%-1.6wt% praseodymium chloride with the samarium trichloride mixed chlorinated rare earth as the fused salt phase, the liquid aluminium lithium alloy of gained of usining mixes it with fused salt mutually as liquid metal, the fused salt phase is 29-35:1 with the volume ratio of liquid metal phase, and the liquid aluminium lithium alloy of take at the uniform velocity stirs 3-7 hour extractive reaction as extraction agent under argon gas atmosphere protection;
C, separation: question response fully after, stop stirring, standing 0.5-1 hour, open purging valve, separates fused salt phase and liquid metal phase, samarium be extracted to liquid metal mutually in and form aluminum-lithium-samarium alloy, praseodymium stay fused salt mutually in, samarium is separated with praseodymium.
2. the method for fused salt according to claim 1 and liquid metal reduction extraction rare-earth separating, is characterized in that: the fused salt phase recycle after separation.
3. the method for fused salt according to claim 1 and 2 and liquid metal reduction extraction rare-earth separating is characterized in that: the described stir speed (S.S.) at the uniform velocity stirred is 60-240 rev/min.
4. the method for fused salt according to claim 1 and 2 and liquid metal reduction extraction rare-earth separating is characterized in that: described LiCl and KCl are respectively 300 ℃, 600 ℃ drying treatment 24 hours.
5. the method for fused salt according to claim 3 and liquid metal reduction extraction rare-earth separating is characterized in that: described LiCl and KCl are respectively 300 ℃, 600 ℃ drying treatment 24 hours.
6. the device of a fused salt and liquid metal reduction extraction rare-earth separating, comprise electrolyzer (3), thermopair (2), anode (1), negative electrode, electrolyzer is placed in pit furnace, it is characterized in that: KCl-LiCl fused salt (4) is housed in electrolyzer, described anode is graphite rod, described negative electrode comprises crucible (6), be loaded on liquid aluminium (5) and molybdenum filament (7) in crucible, the molybdenum filament overcoat has the silica tube bottom to be dipped in liquid aluminium, draw together crucible, anode lower end and thermopair lower end are dipped in fused salt, inflation valve (9) and purging valve (10) are set on pit furnace.
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| CN103728353A (en) * | 2013-12-18 | 2014-04-16 | 中国原子能科学研究院 | Sealed high-temperature electrochemical measuring device |
| CN109777365A (en) * | 2019-01-29 | 2019-05-21 | 云南科威液态金属谷研发有限公司 | A kind of liquid metal composite phase-change energy storage material and its preparation method and application |
| CN112267034A (en) * | 2020-09-08 | 2021-01-26 | 陈毓婷 | Method for producing rare earth |
| CN112921360A (en) * | 2019-12-05 | 2021-06-08 | 乐山有研稀土新材料有限公司 | Method for preparing rare earth metal by molten salt electrolysis |
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| WO2022237513A1 (en) * | 2021-05-08 | 2022-11-17 | 中南大学 | Method for preparing lithium metal by means of molten salt electrolysis |
| CN116875839A (en) * | 2023-09-06 | 2023-10-13 | 山东伟盛铝业有限公司 | Aluminum lithium alloy profile and preparation method thereof |
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| CN103728353A (en) * | 2013-12-18 | 2014-04-16 | 中国原子能科学研究院 | Sealed high-temperature electrochemical measuring device |
| CN103728353B (en) * | 2013-12-18 | 2016-03-30 | 中国原子能科学研究院 | A kind of sealing high-temperature electrochemistry measurement mechanism |
| CN109777365A (en) * | 2019-01-29 | 2019-05-21 | 云南科威液态金属谷研发有限公司 | A kind of liquid metal composite phase-change energy storage material and its preparation method and application |
| CN112921360A (en) * | 2019-12-05 | 2021-06-08 | 乐山有研稀土新材料有限公司 | Method for preparing rare earth metal by molten salt electrolysis |
| CN112921360B (en) * | 2019-12-05 | 2023-01-03 | 乐山有研稀土新材料有限公司 | Method for preparing rare earth metal by molten salt electrolysis |
| CN112267034A (en) * | 2020-09-08 | 2021-01-26 | 陈毓婷 | Method for producing rare earth |
| CN113058296A (en) * | 2021-03-24 | 2021-07-02 | 哈尔滨工程大学 | Plutonium oxalate cup type continuous precipitation device |
| WO2022237513A1 (en) * | 2021-05-08 | 2022-11-17 | 中南大学 | Method for preparing lithium metal by means of molten salt electrolysis |
| WO2024080134A1 (en) * | 2022-10-14 | 2024-04-18 | 京都フュージョニアリング株式会社 | Lithium isotope separation method and lithium isotope separation device |
| CN116875839A (en) * | 2023-09-06 | 2023-10-13 | 山东伟盛铝业有限公司 | Aluminum lithium alloy profile and preparation method thereof |
| CN116875839B (en) * | 2023-09-06 | 2023-12-12 | 山东伟盛铝业有限公司 | Aluminum lithium alloy profile and preparation method thereof |
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