CN103409649B - 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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- CN103409649B CN103409649B CN201310219756.0A CN201310219756A CN103409649B CN 103409649 B CN103409649 B CN 103409649B CN 201310219756 A CN201310219756 A CN 201310219756A CN 103409649 B CN103409649 B CN 103409649B
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- samarium
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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, not only can alleviate that China is near, the pressure of power supply in mid-term anxiety, and has extremely important strategic importance to the long-term stability supply of China's energy and even Sustainable Socioeconomic Development.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 to close to 80GW.Calculate accordingly, China's Nuclear Power Station's Exhausted Fuels accumulation storage capacity will more than 10000 tons when the time comes, and the spent fuel drawn off from Nuclear power plants is every year close to 1700 tons.Effectively utilize the angle with nuclear environment protection from uranium resources, aftertreatment is carried out to spent fuel significant.
Spent fuel post-processing technology can be divided into water law aftertreatment and dry method (mainly referring to molten-salt growth method) aftertreatment two kinds of technology according to the medium used.Dry method post-processing technology is applicable to cooling time is short, burnup is dark thermal reactor spent fuel and the aftertreatment of fast reactor spent fuel fuel, 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, and the component loops that therefore will realize spent fuel utilizes, and 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 vapor transport etc.Current solvent extration has now become the main method of domestic and international Rare Earth Separation, is day by day subject to people's attention the research of its extraction mechanisms and process optimization.Such as number of patent application is 200710098732.9, name is called in the patent document of the processing method of extraction separation of quadravalence cerium, thorium, fluorine and few cerium trivalent rare earth " from the rare earth sulfate solution ", disclose a kind of employing and carry 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 washing of proceed step by step selectivity and back extraction, obtain the method for cerium oxide, Thorotrast, Fluorine contained chemicals.But spent fuel or target piece have the feature of high burnup, high irradiation, this makes traditional water law aftertreatment flow process be difficult to meet separation needs.Do not use water as solvent in the process of dry method aftertreatment (dryreprocessing), its main separating step at high temperature carries out.Flow process has the advantages such as resistance to irradiation, low critical risk, radwaste are few, suitable treatment high burnup, short cooling stage spent fuel.The dry method post-processing technology being medium with fused salt/liquid metal has bright application prospect in spent fuel aftertreatment field.Such as patent publication No. is CN202155172U, name is called in the patent document of " fused-salt extraction stirring paddle device ", openly report the test production that fused salt extraction whipping appts is mainly applicable to radioactivity material, the fields such as abstraction purification, be applied to the mixing of material in its high temperature chemistry, contact, extraction, the aspects such as chemical reaction, for the mixing of applying between the material in pyrochemistry system, reaction etc. provides dynamical foundation and fluid basis, high temperature chemistry is made to realize the mixing of material, contact and then the extraction reached between material, the object such as separation and purification and (or) chemical reaction, also may extend to the test of other pyrochemistries and application in producing.
The present invention is to provide the method for a kind of fused salt/liquid metal reduction extraction rare-earth separating.According to article " the Distribution behavior of uranium of the 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 orbismuth, Journal of Nuclear Materials, 227, 110-121P " middle calculation of distribution coefficient (formula 1, 2) and the method for separation factor (formula 3) calculate the partition ratio of Sm and Pr in alloy and fused salt and separation factor.
β
1=D
Sm/D
Pr(3)
Wherein: D
sm, D
prfor Sm, Pr partition ratio;
be respectively Sm, Pr molar fraction in alloy and fused salt, β
1for the separation factor of samarium and Pr.
Summary of the invention
The object of the present invention is to provide a kind of process simple, can under the extreme condition such as high temperature, severe radiation the fused salt of effective extracting rare-earth element and the method for liquid metal reduction extraction rare-earth separating.The present invention also aims to the device that a kind of fused salt and liquid metal reduction extraction rare-earth separating are provided.
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: employing liquid aluminium is negative electrode, anode adopts spectroscopically pure graphite rod, to join in electrolyzer as ionogen after heat fused, using massfraction at 750-900 DEG C than the KCl-LiCl mixture being 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, add in electrolyzer account for ionogen 0.5%-1.6wt% praseodymium chloride with samarium trichloride mixed chlorinated rare earth as fused salt phase, it is mixed mutually with fused salt using the liquid aluminium lithium alloy of gained as liquid metal, fused salt phase is 29-35:1 with the volume ratio of liquid metal phase, with liquid aluminium lithium alloy for extraction agent at the uniform velocity stirs 3-7 hour extractive reaction under argon gas atmosphere protection;
C, separation: question response completely after, stop stirring, leave standstill 0.5-1 hour, open purging valve, be separated 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 being separated.
2, the described stir speed (S.S.) at the uniform velocity stirred is 60-240 rev/min.
3, described LiCl and KCl is respectively 300 DEG C, 600 DEG C 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, be loaded on liquid aluminium 5 in crucible and molybdenum filament 7, molybdenum filament overcoat has 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, pit furnace is arranged inflation valve 9 and purging valve 10.
What the present invention adopted is that electrolysis fused salt prepares 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 simple substance lithium on liquid cathode aluminium, adds praseodymium chloride and samarium trichloride, carries out following reaction: 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 reaches the object of rare-earth separating.
Feature of the present invention is: (1) adopts fused salt/liquid metal system, relative to the organic solvent of liquid extraction, is applicable to the extreme conditions such as high temperature severe radiation; (2) reductive agent is by fused salt electrolysis, can recycle, economize on resources; (3) volume of material of high-temperature molten salt extraction is little, is conducive to device miniaturization; (4) Sm element is 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 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.
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
Composition graphs 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), and 2, thermopair, 3, corundum crucible; 4, fused salt (eutectic KCl-LiCl); 5, liquid aluminium, 6, monkey, 7, molybdenum filament; 5,6,7 composition negative electrodes; 8 shielding gas (argon gas), 9, inflation valve, 10, purging valve.Concrete operation step: fused salt electrolysis prepares the device of reductive agent as shown in drawings, after obtained liquid aluminium lithium alloy, when 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 molybdenum stirring rake, open inflation valve 9 and be filled with argon gas, inflation rate 3-5L/min.After extractive reaction completes, stop stirring, leave standstill 0.5-1 hour, open purging valve 10, be separated fused salt phase and metallographic phase.
Illustrate below and the method for fused salt of the present invention and liquid metal reduction extraction rare-earth separating be described in more detail:
Prepared by embodiment 1:a, reductive agent: negative electrode adopts liquid aluminium, anode adopts spectroscopically pure graphite rod, using low eutectic KCl-LiCl(massfraction than being 51:43%) mixture to join in electrolyzer after heat fused as ionogen, at 800 DEG C, 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%, obtained liquid aluminium lithium alloy; B, extractive reaction: take out anode and molybdenum filament, with the liquid aluminium lithium alloy of gained for extraction agent, add the PrCl of 0.6wt%
3, the SmCl of 0.6wt%
3, be 29:1 containing the fused salt of mixed chlorinated rare earth and liquid metal phase volume ratio.Open inflation valve, be filled with argon gas, inflation rate 5L/min, under argon gas atmosphere protection, 60 revs/min are stirred 7 hours; C, separation: after question response is complete, stop stirring, leave standstill 1 hour, open purging valve, pour out fused salt, obtain aluminum-lithium-samarium alloy 7.1g.Al, Li, Pr, Sm content in alloy is recorded by ICP, and content is than being 93.1%:2.2%:0.3%:4.4%, and the samarium of 68.1% is extracted in metallographic phase, and partition ratio is 68.1; The praseodymium of 91.5% is stayed in salt, and partition ratio is 2.9, and the separation factor of samarium praseodymium is 23.3.
Prepared by embodiment 2:a, reductive agent: negative electrode adopts liquid aluminium, anode adopts spectroscopically pure graphite rod, using low eutectic KCl-LiCl(massfraction than being 51:43%) mixture to join in electrolyzer after heat fused as ionogen, at 900 DEG C, 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%, obtained liquid aluminium lithium alloy; B, extractive reaction: take out anode and molybdenum filament, with the liquid aluminium lithium alloy of gained for extraction agent, add the PrCl of 1.5wt%
3, the SmCl of 0.8wt%
3, be 35:1 containing the fused salt of mixed chlorinated rare earth and liquid metal phase volume ratio.Open inflation valve, be filled with argon gas, inflation rate 3L/min, under argon gas atmosphere protection, 240 revs/min are stirred 3 hours; C, separation: after question response is complete, stop stirring, leave standstill 0.5 hour, open purging valve, pour out fused salt, obtain aluminum-lithium-samarium alloy 3.7g.Al, Li, Pr, Sm content in alloy is recorded by ICP, and content is than being 84.5%:10.1%:0.9%:4.5%, and the samarium of 61.8% is extracted in metallographic phase, and partition ratio is 115.8; The praseodymium of 94% is stayed in salt, and partition ratio is 23.2, and the separation factor of samarium praseodymium is 5.0.
Prepared by embodiment 3:a, reductive agent: negative electrode adopts liquid aluminium, anode adopts spectroscopically pure graphite rod, using low eutectic KCl-LiCl(massfraction than being 50.5:43%) mixture to join in electrolyzer after heat fused as ionogen, at 900 DEG C, 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%, obtained liquid aluminium lithium alloy; B, extractive reaction: take out anode and molybdenum filament, with the liquid aluminium lithium alloy of gained for extraction agent, add the PrCl of 0.8wt%
3, the SmCl of 1.2wt%
3, be 29:1 containing the fused salt of mixed chlorinated rare earth and liquid metal phase volume ratio.Open inflation valve, be filled with argon gas, inflation rate 5L/min, under argon gas atmosphere protection, 240 revs/min are stirred 3 hours; C, separation: after question response is complete, stop stirring, leave standstill 0.5 hour, open purging valve, pour out fused salt, obtain aluminum-lithium-samarium alloy 4.1g.Al, Li, Pr, Sm content in alloy is recorded by ICP, and content is than being 88.2%:2.0%:1.6%:8.2%, and the samarium of 82.4% is extracted in metallographic phase, partition ratio is 142.3, the praseodymium of 31.1% is stayed in salt, and partition ratio is 13.4, and the separation factor of samarium praseodymium is 10.5.
Claims (6)
1. a method for fused salt and liquid metal reduction extraction rare-earth separating, is characterized in that comprising the steps:
A, prepare reductive agent: adopt 3%-6wt% liquid aluminium to be negative electrode, anode adopts graphite rod, to join in electrolyzer as ionogen after heat fused, using massfraction at 750-900 DEG C than the KCl-LiCl mixture being 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, add in electrolyzer account for ionogen 0.5%-1.6wt% praseodymium chloride with samarium trichloride mixed chlorinated rare earth as fused salt phase, it is mixed mutually with fused salt using the liquid aluminium lithium alloy of gained as liquid metal, fused salt phase is 29-35:1 with the volume ratio of liquid metal phase, with liquid aluminium lithium alloy for extraction agent at the uniform velocity stirs 3-7 hour extractive reaction under argon gas atmosphere protection;
C, separation: question response completely after, stop stirring, leave standstill 0.5-1 hour, open purging valve, be separated 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 is respectively 300 DEG C, 600 DEG C 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 is respectively 300 DEG C, 600 DEG C 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 the liquid aluminium (5) in crucible and molybdenum filament (7), molybdenum filament overcoat has silica tube bottom to be dipped in liquid aluminium, crucible, anode lower end and thermopair lower end are dipped in fused salt, pit furnace is arranged inflation valve (9) and purging valve (10).
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| US5437709A (en) * | 1994-07-26 | 1995-08-01 | Iowa State University Research Foundation, Inc. | Recycling of rare earth metals from rare earth-transition metal alloy scrap by liquid metal extraction |
| CN1468979A (en) * | 2002-07-19 | 2004-01-21 | 中国地质科学院成都矿产综合利用研究 | Oxide and salt melt electrolyzing process of producing cell-level mixed RF metals |
| CN1198000C (en) * | 2002-11-08 | 2005-04-20 | 包头市长河稀土材料有限公司 | Lanthanum and cerium composite alloy additive and preparing method thereof |
| CN101319275B (en) * | 2007-06-04 | 2010-11-10 | 北京有色金属研究总院 | Process for solvent extraction separation purification of rare earth element |
| CN101994004B (en) * | 2009-08-11 | 2012-07-11 | 北京有色金属研究总院 | Process for extracting and separating rare-earth elements |
| CN102011020B (en) * | 2009-12-14 | 2012-09-05 | 包头市玺骏稀土有限责任公司 | Method for recovering rare earth elements from neodymium-iron-boron wastes |
| CN102691077A (en) * | 2012-06-15 | 2012-09-26 | 徐州金石彭源稀土材料厂 | Process for extracting praseodymium from rare earth |
| CN102719674A (en) * | 2012-07-13 | 2012-10-10 | 赣县金鹰稀土实业有限公司 | Method for extracting rare earth from oxidized neodymium iron boron waste |
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| EP3339480A1 (en) | 2016-12-21 | 2018-06-27 | Sintef TTO AS | Electrochemical production of rare earth alloys and metals comprising a liquid anode |
| WO2018114925A1 (en) | 2016-12-21 | 2018-06-28 | Sintef Tto As | Electrochemical production of rare earth alloys and metals comprising a submerged liquid anode |
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