Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D11/00—Solvent extraction
  • B01D11/04—Solvent extraction of solutions which are liquid
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D11/00—Solvent extraction
  • B01D11/04—Solvent extraction of solutions which are liquid
  • B01D11/0426—Counter-current multistage extraction towers in a vertical or sloping position
  • B01D11/043—Counter-current multistage extraction towers in a vertical or sloping position with stationary contacting elements, sieve plates or loose contacting elements
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D11/00—Solvent extraction
  • B01D11/04—Solvent extraction of solutions which are liquid
  • B01D11/0476—Moving receptacles, e.g. rotating receptacles
• • G—PHYSICS
  • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
  • G21C—NUCLEAR REACTORS
  • G21C19/00—Arrangements for treating, for handling, or for facilitating the handling of, fuel or other materials which are used within the reactor, e.g. within its pressure vessel
  • G21C19/42—Reprocessing of irradiated fuel
  • G21C19/44—Reprocessing of irradiated fuel of irradiated solid fuel
  • G21C19/48—Non-aqueous processes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
  • B01D35/28—Strainers not provided for elsewhere
• • C—CHEMISTRY; METALLURGY
  • C21—METALLURGY OF IRON
  • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
  • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
  • C21C7/04—Removing impurities by adding a treating agent
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E30/00—Energy generation of nuclear origin
  • Y02E30/30—Nuclear fission reactors
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
  • Y02W30/00—Technologies for solid waste management
  • Y02W30/50—Reuse, recycling or recovery technologies

Definitions

• the invention relates to a method and a device for bringing into contact without mixing two immiscible liquids.
• the invention relates to a method and a device for bringing metals and molten salts into contact at high temperatures which can reach, for example, up to 800 ° C.
• the technical field of the invention can be defined generally as that of material transfer more particularly, that of chemical contacting and separation techniques and more particularly of extraction involving immiscible liquids.
• the technical field of the invention is more precisely but not exclusively that of high temperature liquid / liquid extraction systems also known as pyrocontacters in which a liquid salt phase and a molten metal phase are brought into contact.
• Documents [1-2] describe bulk packing columns, or a tray column using the molten chloride / bismuth system.
• the use of the extraction columns described in these documents is limited by exchange kinetics.
• the HEPT (theoretical equivalent height) of these columns is generally between 1 and 2 m.
• the document [3] describes a rotary packing column which is used in particular for bringing into contact a phase of molten potassium chloride-aluminum chloride salts containing plutonium and a uranium-aluminum alloy.
• Document [5] describes a centrifugal pyrocontactor for mixing and then separating liquid salts and immiscible liquid metals.
• the liquids are introduced into an annular mixing zone and are vigorously mixed using vertical blades attached to a rotor associated with deflectors.
• the liquids are introduced into the apparatus at a temperature of 700 to 800 ° C. and are separated in the rotor in a dense phase and in a light phase which are removed from the apparatus.
• This apparatus is used to treat molten chloride baths resulting from an electrorefining process.
• centrifugal extractor described in this document is a powerful device but has been tested for low periods of time not exceeding a few hundred hours in molten chloride medium. Its reliability has therefore not been proven for a sufficient length of time. The use of these devices is also limited by the appearance of corrosion problems that quickly alter their operation.
• the object of the invention is to provide a method and a device for bringing into contact two immiscible liquids which meet these needs, among others.
• the object of the invention is still to provide such a method and such a device which do not have the disadvantages, defects, limitations and disadvantages of the methods and devices of the prior art and which solve the problems of the methods and devices of the invention. prior art.
• a method of bringing into contact without mixing a first liquid and a second immiscible liquid in which the following successive steps are carried out: -a) placing the first liquid in at least one container comprising a wall of a solid material non-reactive vis-à-vis the first and second liquids, said wall comprising one or more orifices through; the first liquid being non-wetting vis-à-vis said solid material of the wall;
• the first liquid is left in contact with the second liquid for a time sufficient for an exchange, transfer of material, between the first and second liquids; d) removing said first container from the volume of the second liquid.
• the densities of the first and second liquids are close.
• close densities it is generally meant that the two densities of the first and second liquids do not differ by more than 10%, preferably not more than 5%, more preferably not more than 1%.
• the first liquid is non-wetting with respect to the material of the wall, which means that generally its contact angle ⁇ with said wall is greater than 90 °, preferably it is between 120 and 180 °.
• the second liquid may be wetting or non-wetting, but it must preferably have a rather wetting character vis-à-vis the material of the dividing wall.
• the method according to the invention is simple, reliable, easy to implement. It meets the needs and requirements listed above and provides a solution to the problems of the prior art mentioned above.
• the method according to the invention can be implemented easily regardless of the nature of the liquids in contact and the temperature for example when it comes to metals or molten salts.
• the method according to the invention is effective and involves a minimum of movements, transfers of the two liquids.
• the process according to the invention can be carried out in a relatively short time, for example between 3 and 24 hours, because the contact surface of the open crucibles makes it possible to reach thermodynamic equilibrium in a short time.
• the sufficient duration of the contacting of step c) can be easily determined by the skilled person in this field of the art and is generally from 2 to 10 minutes, and can reach for example up to 1 hour.
• the method according to the invention can be carried out both in discontinuous mode of operation and in a continuous mode of operation.
• the first liquid / second liquid / solid material interfacial tension of the wall is high.
• the interfacial tension first liquid / second liquid / solid material of the wall is greater than 0.3 N. m 1 , preferably greater than 0.6 N. m -1 .
• the first liquid has a surface tension greater than 0.3 N.m -1 , preferably greater than 0.8 N.m -1 .
• the first liquid may be a pure metal or an alloy of several molten metals.
• the said metal or metals may be chosen for example from aluminum and copper.
• the second liquid particularly in the case where the first liquid is constituted by one or more molten metals, may consist of a molten salt or a mixture of several molten salts.
• these molten salts are generally chosen from alkali metal, alkaline earth metal or aluminum chlorides, for example LiCl, AlCl 3; and fluorides of alkali, alkaline earth metal, or aluminum such as LiF, AlF 3 .
• the first liquid may also be selected from water and water / alcohol solutions and the second liquid may be selected from paraffin oils.
• steps b) to d) can be repeated, that is to say that the container is then immersed again in a volume of a third liquid which is different from the second liquid.
• the transfer (exchange) of material carried out during step c) may be any material transfer operation that can take place between two liquids, preferably said transfer of material is a liquid / liquid extraction during which one of the components of the second liquid passes into the first liquid and / or one of the constituents of the first liquid passes into the second liquid.
• said first liquid may be molten aluminum and the second liquid may comprise molten fluoride salts containing aluminum fluoride, and in which one or more several actinide fluorides and one or more lanthanide fluorides; and in step c), said actinide fluorides are reduced chemically by contact with the molten aluminum to said actinides (in the form of metals) which consequently go into solution in the first liquid, whereas the lanthanide fluorides (non-reactive) remain in the second liquid.
• steps b) to d) can then be repeated by immersing the at least one container containing the aluminum and the actinides (metals) in a volume.
• a third liquid consisting of one or more melted alkali or alkaline-earth metal chlorides containing aluminum chloride, whereby the actinides are chemically oxidized by contact with said fluorides melted into actinide chlorides which pass into the third liquid (in the oxidized form of chlorides); and the molten aluminum is regenerated and can optionally be reused for a new extraction / desextraction cycle.
• Step b) of the process of the invention is preferably carried out under a primary vacuum of 2 ⁇ 10 -2 to 10 -1 mbar absolute when the two liquids are brought into contact, which guarantees an "intimate" contact between the two liquids. that is to say that said gas pocket can be intercalated between the two phases and is eliminated.
• step c) of the process according to the invention is carried out, preferably under an inert gas atmosphere such as Argon, preferably at a pressure close to atmospheric pressure, in particular to avoid salt evaporation. molten.
• an inert gas atmosphere such as Argon
• the invention furthermore relates to a device for carrying out the method as described above, this device comprises: one or more first receptacles intended to receive a first liquid and comprising a wall made of a solid material that is non-reactive vis-à-vis screw first and second immiscible liquids, said wall including one or more through-holes, the first liquid being non-wetting with respect to said solid material of the wall; a second container intended to receive a volume of a second liquid; means for supporting the container (s) containing the first liquid so as to immerse them in said volume of the second liquid and then remove them from the volume of the second liquid.
• the device according to the invention has all the advantages, effects, related to the implementation of the method according to the invention. It is particularly simple, reliable, and it has a minimum of moving parts for maximum efficiency. Its energy consumption is minimal. It can be designed to be easily remote controlled to be implemented in nuclear containment for example shielded type box.
• the one or more containers are generally made of a material chosen as a function of these holding properties with respect to the experimental conditions as well as of its character of non-wettability with respect to the first liquid. They can thus be made of a material chosen from graphite and boron nitride.
• the container (s) may be cylindrical in shape with a circular cross-section having side walls and a bottom or bottom wall.
• this bottom has a rounded geometry to avoid the presence of dead volumes allowing a diffusion of the second liquid under the first in other words in order to limit the possible accumulation of the second liquid.
• Said openings, openings have a cross-sectional shape that can be chosen from circles, polygons such as squares, rectangles, in particular rectangles whose length / width ratio is high.
• a preferred form for said orifices, especially in the case where the first containers are cylindrical containers is that of slots made in the bottom of said containers and which extend along the side walls of said containers.
• the means for supporting said first containers, immersing them in said volume of the second liquid and removing them from said volume of the second liquid may comprise a vertical rod at the lower end of which is fixed an element supporting the first containers.
• Said element supporting the first containers may have the shape of a carousel or circular barrel, comprising a central axis located in the extension of said vertical rod, said containers being arranged in a circle concentric to the central axis of said carousel or barrel.
• the at least one container may be secured to the container support member by any known means such as keys.
• said support element of the first containers may comprise at its center a preferably cylindrical part making protruding downwardly beyond the base of said first containers and to control the depth of immersion, limit the dead volume in the container containing the second liquid and finally to bring a cold point to allow a movement of the second liquid by thermal convection.
• the device is placed in a furnace, for example a well-type furnace, and the upper end of the vertical rod is preferably located outside the furnace. oven to allow handling, and possibly forming a cold source.
• FIG. 1 is a sectional side view of a device according to the invention such as a pyrocontactor, comprising perforated baskets immersed in a liquid medium such as molten salts;
• Figure 2 is a top view of the barrel, carousel, of the device of Figure 1 equipped with six perforated baskets;
• FIG. 3 is a perspective view of the barrel, carousel, of the device of FIG. 1 equipped with six perforated baskets with openings of different geometries;
• FIG. 4 is a sectional side view of one of the perforated baskets of the carousel barrel of Figures 1, 2, 3;
• FIG. 5 is a diagrammatic sectional view showing the contact angle ⁇ of the "triple" point defined between the first liquid (medium 1), the gaseous atmosphere prevailing in the furnace such as argon and the solid wall; one of the openwork baskets at one of the slits of this basket;
• FIG. 6 is a diagrammatic sectional view showing the contact angle ⁇ 'at the triple point defined between the first liquid (medium 1), the second liquid (medium 2) and the solid wall of one of the perforated baskets at the from one of the slots in this basket.
• the device shown in Figure 1 comprises first a container, crucible (1) of a material such as graphite, boron nitride or other when it is put into contact with liquids at high temperature.
• This crucible (1) is intended to receive one of the liquids (second liquid) (2) which may consist of one or more mixed melted salts.
• molten salts may in particular be chlorides or molten fluorides.
• the device of FIG. 1 can in particular be used to allow the group extraction of actinides such as uranium, plutonium, americium, curium contained in a solution of molten fluorides and which are reduced in their metallic form in contact with aluminum metal. fusion contained in the baskets added.
• the second liquid such as the salt (s) melted (s) rise to a level (3) in the crucible (1).
• the device as described in Figure 1 is then placed in a heater such as a furnace (not shown).
• the device according to the invention in the embodiment of FIG. 1 comprises a plurality of perforated perforated baskets (4) which contain the
• perforated baskets (4) are attached to a support element, which may be called carousel or barrel (6).
• the carousel barrel (6) supports six baskets, perforated, perforated
• Such a carousel can support for example from 1 to 6 basket (s), it is then necessary to replace the basket or basket (s) not used (s) by a corresponding number of basket material full
• the carousel, barrel, (6) basket holder also includes a central part or piece
• the barrel system, carousel, illustrated allows to quickly change the type and nature of openwork baskets, each of which is supported by a simple key.
• the part, or piece, central (7) of the carousel (6) is recessed (8) and can optionally receive a thermocouple and / or a thermal bridge.
• a metal rod (9) can thus be placed for these purposes in this central recessed portion (8) of the carousel, barrel (6).
• the central part portion of the support of perforated baskets, or barrel or carousel (6) is immersed in the "second" liquid such as molten salts to cause local cooling of the liquid, a few degrees.
• the rod (9) and the projecting central portion (7) thus create a thermal bridge between the inside and the outside of the oven. This results in a temperature gradient between the central portion of the second colder liquid and the edge of the crucible hotter because in contact with the furnace, which causes a free convection current.
• the currents of convection are all the more important as the temperature gradient is high and the conductivity thermal liquid medium consisting of the second liquid is low.
• the submerged central piece (7) also has the advantage of reducing the "dead" volume in the crucible containing the second liquid such as molten salts. Such a design makes it possible to obtain a ratio of the volume of the perforated baskets to the volume of the crucible close to 1.
• the central piece (7) also makes it possible to provide a safety stop and to control the height positioning of the carousel in the temperature system, that is to say in the system brought to the working temperature, which is in particular a temperature ensuring the melting of the metal phases and salts of each of the respective liquids.
• the modification of the geometry of the submerged central part (7) makes it possible to change the volume or mass ratio of the phases in contact and to optimize the operating conditions of the process.
• the submerged central portion (7) of the barrel or carousel may have a star geometry or a polygon geometry.
• the assembly constituted by the barrel, carousel and perforated baskets is held in the rod (18) with the aid of pins.
• the upper part of the carousel penetrates into the annular space of the inconel rod (18) and (19) and is thus held in a fixed position.
• the rod which can be described as lifting rod, and which equips the oven, such as a furnace, in which is placed in the device according to the invention can raise and move the carousel and baskets which they are fixed to immerse it in different liquid media, for example different solutions of molten salts.
• the holding rod (18) (19) of the assembly formed by the barrel and the baskets can be connected to a remote rotation system, which thus allows dynamic mixing of the liquid medium contained in the crucible.
• the implementation of such brewing increases the efficiency of the device.
• the perforated baskets (4), as shown in FIG. 3, have a generally cylindrical shape, generally of circular cross-section, with an open top (10), and their bottom wall or bottom (11) is preferably provided with an internal rounded machining (12) which avoids any dead volume, and therefore the accumulation of the second liquid.
• connection between the side walls (13) of the basket (4) and the bottom (11) thereof is via a rounded wall portion.
• the perforated baskets can however also be closed in their upper part to avoid any contamination of the liquid contained therein to a level (14), such as molten metal, by the vapors and condensates from the second liquid phase, for example molten salts, contained in the "lower" crucible .
• the closure of the baskets can also be achieved by solidification, in the upper part, of the liquid contained in the basket.
• the wall and bottom of the baskets are, according to the invention, made of an inert material that is non-reactive with respect to the two liquids.
• first liquid is made of a liquid metal
• second liquid is constituted by molten salts - for example in the case of a contact extraction between molten Ai and molten fluorides, then a contact de-extraction between molten Ai and molten chlorides - the material chosen may be graphite.
• the said material may also be coated with a protective layer made of pyrocarbon, or boron nitride.
• the choice of materials for the wall of the baskets is much wider: it may be in particular glass , pyrex or even selected polymeric materials, in particular, depending on their hydrophilic or lipophilic nature.
• the condition of low wettability of this material by the first liquid or liquid 1 (content), expressed by an angle ⁇ greater than 90 °, must of course be respected.
• the device according to the invention based on the implementation of perforated baskets can be used in wide temperature ranges ranging for example from room temperature to 1000 0 C, or even beyond by choosing the materials. adequate.
• the walls (including the bottom) of the basket or baskets are provided with orifices, openings (15), at the level of which the contact occurs, without mixing, between the first liquid phase contained inside. baskets, perforated, pierced, perforated and the second liquid phase which is outside these baskets in the crucible.
• the number, the position, the geometry and the size of the openings (15) of the baskets can be modified to allow in particular an adjustment of the contact surface between the two liquid media. For example, these modifications can improve the exchange kinetics of a liquid / liquid extraction process. Other geometric modifications may be made to limit the retention of liquids in the perforated baskets, at their openings, during the medium change operations during the extraction and de-extraction steps.
• the openings may have, in section, the shape of circles, squares, polygons such as rectangles, preferably elongated rectangles that is to say slits; these openings may be provided both on the side walls and on the bottoms of containers such as cylinders.
• openings are visible in Figures 2 and 3 or the six baskets carried by the carousel each have openings of different shapes in different numbers.
• all baskets can have openings of the same shape and the same number for ease of handling and movement.
• the circular openings will have a diameter of 1 mm and the slots will have a length of 19 mm and a width of 1 mm.
• the shape of the openings of the baskets shown in FIG. 4 which are constituted by slits, windows (16) perforated with a width for example of 1 mm starting in the base wall of the basket at an interval by example of 0.8 cm from the edge and for example up to 15 mm high on the side wall (13) (for cylindrical baskets having for example a height of 100 mm and a diameter of 21.5 mm ), allows evacuation of the gas bubbles during contacting the two melts under a controlled atmosphere.
• This particular configuration of the openings has an improvement over perforated baskets having openings of simple shape such as circles.
• one of the two liquids preferably the one inside the perforated baskets
• has a high surface tension value namely a surface tension greater than 0, 3 Nm "1, that is the case, for example molten aluminum at 933K [8] which has a surface tension value of 0.87 Nm" 1.
• the surface tension is that which prevails on the surface of the liquid or rather at the interface between said liquid and the gaseous atmosphere prevailing in the furnace.
• the unit of surface tension (N. m- 1 ) is equivalent to joules per square meter (J. m- 2 ), which corresponds to one unit of surface energy.
• Such a characteristic is important because it makes it possible to preserve the first liquid in the baskets, without any loss, flow, during the movements of the baskets (by lifting with the metal rod of the furnace, well described above) in the atmosphere for example furnace argon between the immersions in the different liquid media, such as molten salts, used to carry out, for example, the extraction steps of the actinides present in the fluoride solutions, followed respectively by the extraction of the medium melted chlorides.
• the different liquid media such as molten salts
• the maximum hydrostatic height corresponds to the maximum height of the column of the first liquid that can be received in a perforated basket implemented according to the invention, this hydrostatic height is in particular a function of the geometry of the orifices, openings of this basket.
• the maximum hydrostatic height can be calculated in two cases: the first is where the baskets are raised, not immersed and where the first liquid or liquid "1" such as the molten Ai contained in these baskets is in contact with the gas such as argon constituting the furnace atmosphere.
• the second case is where the perforated baskets are lowered, immersed in the second (or third) liquid such as molten salts.
• This maximum hydrostatic height can be calculated in the first case using a Young-Laplace equation that can be described as a simplified Young-Laplace equation, where surface tension is applied to the surface.
• liquid or rather at the interface between the liquid "1" contained in the basket such as molten aluminum and the gaseous atmosphere prevailing in the oven during the steps of raising and moving the baskets.
• This atmosphere consists for example of a primary vacuum or Ar ( Figure 5).
• Equation No. 1 makes it possible to size apertures of perforated baskets making it possible to contain different heights, of first liquid, for example molten Al, without against pressure of a liquid such as a molten salt. Examples of opening geometries are given in Table No. 1 below for Ai contained in a graphite crucible, taking into account an interfacial tension value of 0.87 N. m- 1 :
• the method and the device according to the invention as described above may be implemented to perform any material transfer operation between two liquids.
• This operation may especially be a liquid / liquid extraction operation and more particularly a liquid / liquid extraction operation at high temperature.
• pyrocontactor we will then speak of a pyrometallurgical process and the apparatus according to the invention will then be called pyrocontactor.
• This pyrometallurgical process and this pyrocontactor device find their application particularly in the field of reprocessing spent nuclear fuel.
• the pyrocontactor allows the group extraction of actinides contained in a molten fluoride solution such as LiF / AlF 3 .
• the placing in contact between the molten salts, for example LiF / AlF 3, and the perforated baskets, containing a molten metal such as molten aluminum makes it possible to chemically reduce the actinides initially in their fluoride form to their metallic form and to recover them. in the aluminum phase.
• the contact time between the two liquid phases is between a few minutes and a few hours.
• the pyrocontactor avoids the mixing of saline and metallic phases.
• the pyrocontactor can again be positioned in the starting salt bath containing a new fuel charge to be reprocessed.
• the liquid such as Al placed in the perforated baskets can be recycled at the end of the de-extraction step.
• the basket system acts as a "chemical” pump because the extractant compound is never consumed in the process.
• This "chemical” pump makes it possible to extract and return one or more compounds in solution without using a gravitational or accelerating field, as is the case when settling or centrifugation is being carried out. separate the phases put in contact.
• This feature facilitates the implementation of extraction and represents a real interest for high temperature processes. Controlling the thermal equipment also improves the kinetics of extraction by setting up a free convection solution mixing controlled (and not forced). Indeed, the free convection can be controlled by the establishment of a cold source provided in (7) and / or (9).
• the geometry of the proposed system ( Figure 1) allows, for example, a practical implementation in a well-type furnace (not shown).
• the crucible where the second liquid, such as molten salts, can be closed at its upper part by an insulating cover (17).
• This cover (17) is traversed by a double envelope rod sectional view along (18) and (19).
• At the crossing of the lid are provided holes (20) for fixing on the outer casing of the rod (19) which allow the positioning in height, using keys, of the entire carousel pyrocontactor.
• the device according to the invention as described for example in Figure 1 can operate in a discontinuous mode particularly well suited for use in a shielded box with small amounts of material (for example 100 to 1000 g of molten salts and molten metal ).
• small amounts of material for example 100 to 1000 g of molten salts and molten metal .
• the implementation of larger quantities may however be possible provided that adaptations are made to allow continuous operation.
• the procedure consisted in dissolving 10 g of NdF 3 in 300 g of LiF / AlF 3 .
• the salt mixture thus obtained was placed in the graphite crucible with a capacity of 11 and then melted in a "well” oven at a temperature of 700 to 800 ° C.
• the contact between the salt and molten metal media is then carried out under a primary vacuum, before placing the inside of the oven under Ar at atmospheric pressure in order to avoid any phenomenon of excessive evaporation of the salt.
• the carousel rack containing the 6 baskets is raised slowly at a rate of 10 cm every 1 / 2h to allow a good drip of molten salt in the melting zone of the oven.
• the system fig.3 is positioned in the upper part of the oven to allow the cooling of the baskets.
• the cooling of the assembly can be accelerated by conducting an argon sweep at 20 0 C at the head of the raised pyrocontactor.
• the heights of Al thus put in place are between 1.5 and 8 cm.
• the weight loss measurements made on each crucible showed weight variations of the order of 0.5%. This good result validated the possibility of maintain the liquid Al in an Ar atmosphere without the hydrostatic pressure of a molten salt.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Physics & Mathematics (AREA)
• Engineering & Computer Science (AREA)
• Plasma & Fusion (AREA)
• General Engineering & Computer Science (AREA)
• High Energy & Nuclear Physics (AREA)
• Manufacture And Refinement Of Metals (AREA)
• Extraction Or Liquid Replacement (AREA)
• Physical Or Chemical Processes And Apparatus (AREA)

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• 2006
  • 2006-12-21 FR FR0655829A patent/FR2910344B1/fr active Active
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