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EP3370855B1 - Vorrichtung zum mischen von pulvern mit kryogenem fluid und verfahren - Google Patents

Vorrichtung zum mischen von pulvern mit kryogenem fluid und verfahren Download PDF

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Publication number
EP3370855B1
EP3370855B1 EP16791565.1A EP16791565A EP3370855B1 EP 3370855 B1 EP3370855 B1 EP 3370855B1 EP 16791565 A EP16791565 A EP 16791565A EP 3370855 B1 EP3370855 B1 EP 3370855B1
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EP
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Prior art keywords
powders
mixing
passage
chambers
cryogenic fluid
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English (en)
French (fr)
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EP3370855A1 (de
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Méryl BROTHIER
Stéphane VAUDEZ
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/60—Mixing solids with solids
    • B01F23/66—Mixing solids with solids by evaporating or liquefying at least one of the components; using a fluid which is evaporated after mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/51—Methods thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/53—Mixing liquids with solids using driven stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/55—Mixing liquids with solids the mixture being submitted to electrical, sonic or similar energy
    • B01F23/551—Mixing liquids with solids the mixture being submitted to electrical, sonic or similar energy using vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/60—Mixing solids with solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/60—Mixing solids with solids
    • B01F23/69—Mixing systems, i.e. flow charts or diagrams; Arrangements, e.g. comprising controlling means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/70—Pre-treatment of the materials to be mixed
    • B01F23/705—Submitting materials to electrical energy fields to charge or ionize them
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
    • B01F25/452—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces
    • B01F25/4523—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces the components being pressed through sieves, screens or meshes which obstruct the whole diameter of the tube
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/11—Stirrers characterised by the configuration of the stirrers
    • B01F27/19—Stirrers with two or more mixing elements mounted in sequence on the same axis
    • B01F27/191—Stirrers with two or more mixing elements mounted in sequence on the same axis with similar elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
    • B01F27/61—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis about an inclined axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • B01F31/83—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations comprising a supplementary stirring element
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • B01F31/86—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations with vibration of the receptacle or part of it
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/05—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material
    • B01F33/052—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material the energy being electric fields for electrostatically charging of the ingredients or compositions for mixing them
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
    • B01F33/811—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles in two or more consecutive, i.e. successive, mixing receptacles or being consecutively arranged
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/75—Discharge mechanisms
    • B01F35/754—Discharge mechanisms characterised by the means for discharging the components from the mixer
    • B01F35/7547—Discharge mechanisms characterised by the means for discharging the components from the mixer using valves, gates, orifices or openings
    • B01F35/75471—Discharge mechanisms characterised by the means for discharging the components from the mixer using valves, gates, orifices or openings being adjustable
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/57—Mixing radioactive materials, e.g. nuclear materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/58—Mixing liquids with solids characterised by the nature of the liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/834—Mixing in several steps, e.g. successive steps

Definitions

  • the present invention relates to the field of the preparation of granular media, and more specifically to the mixture of powders, in particular actinide powders, and to their deagglomeration / reagglomeration to obtain a mixture of high homogeneity by means of a cryogenic fluid , also called median cryogenic.
  • a cryogenic fluid also called median cryogenic.
  • the invention thus preferably has its application for the mixture of actinide powders for the formation of nuclear fuel, in particular nuclear fuel pellets.
  • the invention thus proposes a device for mixing powders by cryogenic fluid, as well as a method for mixing powders associated with it.
  • the implementation of the various stages of preparation of a granular medium, in particular from actinide powders, to form nuclear fuel pellets after forming by pressing, is essential because it mainly determines the control of the microstructure of the substrate. final product but also the presence or absence of defects of macroscopic aspects within a fuel pellet.
  • the mixture of actinide powders to allow the production of nuclear fuel is a key step in controlling the quality of the fuel pellet obtained, which is most often subject to compliance with stringent requirements in terms of microstructure and impurities.
  • the mixer in dry phase without internal media. It may in particular be a Turbula® type mixer from the company WAB which by more or less complex movements of the tank containing the powders to be mixed, allows more or less homogenization of the granular medium.
  • WAB Turbula® type mixer
  • the efficiency of this type of mixer is limited. Indeed, depending on the type of powders to be mixed, there may remain heterogeneous areas, for which mixing does not occur or at least in an incorrect manner and not admissible.
  • the kinematics of this type of mixer is generally not complex enough to induce a thorough mixture, that is to say a mixture that is satisfactory in terms of homogeneity, without focusing itself, or a penalizing mixing time. at the industrial level.
  • the energy transmitted to the granular medium in this type of mixer does not allow deagglomeration to be sufficient to reach sufficient degrees of homogeneity in the case where the size of these agglomerates is too large (in particular to be compensated during the sintering step).
  • the principle of the media mixer is also known. According to this principle and to promote the mixing operation, one or more mobile can be used within the tank containing the powder to be mixed. These mobiles can be blades, turbines, shares, ribbons, worms, among others. To improve the mixing, the tank can itself be mobile. This type of mixer may be more efficient than the previous category but is still insufficient and suffers limitations. In fact, the stirring induces a modification of the granular medium by agglomeration or deagglomeration which is difficult to control, which induces a proliferation of powders and / or a degradation of the flowability of the granular medium.
  • the use of mobile (media) for mixing causes pollution (contaminations) when it comes to mixing abrasive powders such as those to be implemented for the realization of nuclear fuel.
  • the mobiles implemented induce retentions that generate very high dose rates in the case of the development of nuclear fuel.
  • the aforementioned mixers are not fully satisfactory for mixing certain powders, such as actinide powders, and it is necessary to carry out a granulation step in order to obtain a flowable granular medium.
  • mixers are also known, implementing a multiphasic medium, namely fluid-solid phases. These mixers can be classified in two main categories described below.
  • liquid / solid type mixers there are liquid / solid type mixers. These mixers are not effective for the implementation of soluble powders with the liquid phase used in the mixer or if the powders are modified by contact with the fluid. Moreover, for powders having a high density compared to the liquid introduced into the mixer, the mixture is most often not effective or requires significant stirring speeds. Indeed, the take-off speed of a particle from the bottom of the agitator is directly related to the density difference between the particles constituting the powders and that of the liquid for suspending. In this case, it can be used viscous liquids but this induces an increased energy demand, and this in proportion to the increase in viscosity before reaching a turbulent regime to promote mixing.
  • the constituent particles of the powders to be mixed have relatively small diameters, typically less than 10 microns, it is not conceivable to make homogeneous and complete suspensions with this type of device without using complementary mixing means.
  • technologies such as that described in the patent application CA 2 882 302 A1 have been proposed but remain nevertheless inoperative for a mixture of actinide powders, the vibration means used not allowing sufficient homogenization in view of the objectives of homogenization to achieve and the particularities of the actinide powders.
  • the volume of the mixer must be limited, to prevent any risk of double loading that could lead to exceeding the critical mass allowable. Indeed, in a conventional liquid / solid mixer, the particle density per volume of The tank can not be large unless it exceeds a stirring power that is too high, or undergoes slow mixing kinetics.
  • liquid phase powder mixers in particular of the type described in the patent applications CA 2 882 302 A1 , WO 2006/0111266 A1 and WO 1999/010092 A1 , are not suitable for the problematic of a mixture of powders of actinide powders type, since they would require too great stirring speeds to hope to take off the powders from the bottom of the stirring tank and reach levels of consistent with those sought in the nuclear industry. In addition, once again, they would induce contaminated effluents, difficult to manage industrially but also risks of criticality or even radiolysis of the liquid phase used because of the nature of the powders to be used (beyond the fact that these can interact chemically with the liquid used).
  • the object of the invention is to at least partially remedy the needs mentioned above and the drawbacks relating to the embodiments of the prior art.
  • a cryogenic fluid here designates a liquefied gas kept in the liquid state at low temperature.
  • This liquefied gas is chemically inert under the conditions of implementation of the invention for the powders to be mixed and deagglomerated.
  • the powder mixing device according to the invention may further comprise one or more of the following characteristics taken separately or in any possible technical combinations.
  • the cryogenic fluid may comprise a weakly hydrogenated liquid, ie a liquid comprising at most one hydrogen atom per molecule of liquid, having a boiling point lower than that of water.
  • the device may comprise means for mixing the mixing chamber according to a gyroscopic movement.
  • the mixing means according to a gyroscopic type of movement can allow the movement of the mixing chamber, even the rotation, along the three axes of the three-dimensional metrology.
  • This type of agitation by gyroscopic movement may in particular allow to promote the mixing of the powders when they have high densities compared to the density of the fluid phase of the cryogenic fluid located in the mixing chamber.
  • Each mixing chamber may then comprise a cryogenic fluid, in particular being filled with a cryogenic fluid, and stirring means, in particular being equipped with stirring means, to allow mixing of the powders placed in suspension in the cryogenic fluid.
  • the stirring means may comprise mixing mobiles, in particular blades, turbines and / or duvet mobiles, among others.
  • These mixing mobiles may comprise grinding mobiles, for example of the type balls, pebbles, among others.
  • the stirring means may also comprise means for generating vibrations, in particular ultrasonic vibrations, in particular sonotrodes.
  • passage restriction systems may include sieves.
  • the passage restriction systems may further include diaphragms.
  • the passage restricting systems may be adjustable and configured so that their passage cross-section decreases as a function of the flow of powder flow through the plurality of mixing chambers, the passage section of a (n-1)
  • the passage restriction system is thus greater than the passage section of an nth passage restriction system by following the flow flow of the powders.
  • passage section of the passage restriction systems may be smaller than the natural flow section of the powders, so that these powders are necessarily deagglomerate when they pass from one mixing chamber to the other .
  • the residence time of the particles to be mixed is intrinsically sufficient to allow disagglomeration.
  • the plurality of mixing chambers and the plurality of powder passage restriction systems may advantageously be arranged in the same vertical direction so as to allow the powder to flow under the effect of gravity.
  • the device preferably comprises a system for electrostatically charging the powders intended to be introduced into the mixing chamber or chambers.
  • Part of the powders may in particular be brought into contact with one part of the electrostatic charge system to be electrostatically charged in a positive manner and the other part of the powders may be brought into contact with the other part of the electrostatic charge system to be charged. Electrostatically negative, to allow differentiated local agglomeration. When mixing more than two types of powders, some powders may be either positively charged, or negatively charged, or without charge.
  • the cryogenic fluid may also be of any type, in particular being liquefied nitrogen or argon. It should be noted that the use of nitrogen is relevant because of its low price but also because the glove boxes and the processes used for the development of the plutonium-based nuclear fuel are inert to the environment. nitrogen and that liquid nitrogen is itself used in some fuel operations (BET measurement, ). The use of this type of cryogenic fluid does not therefore induce any additional particular risk in the production process.
  • the device may especially comprise at least two powder supply enclosures, and in particular as many powder supply enclosures as types of powders to mix.
  • the supply enclosure (s) may comprise adjustable feed hoppers and / or metering type systems, especially trays or vibrating corridors.
  • the powders can advantageously be electrostatically charged in a different manner, in particular in an opposite manner in the presence of at least two types of powders, to promote differentiated local agglomeration.
  • the device may comprise a single mixing chamber, and said mixing chamber may be animated with a gyroscopic type of movement to allow mixing of the powders.
  • the device may comprise a plurality of powder mixing enclosures, successively arranged in series one after the other, or the powder supply enclosures for introducing the powders into the minus the first mixing chamber, and a plurality of powder passage restriction systems, each passage restriction system being located between two successive mixing chambers, to constrain the distribution of powders from one mixing chamber to the next, each mixing chamber comprising a cryogenic fluid and stirring means to allow mixing of the powders suspended in the cryogenic fluid, the process then possibly comprising the step of progressively restricting the passage of the flow of the powders through mixing enclosures through p-section passage restriction systems decreasing wettage according to the flow of the powders.
  • the device and method for mixing powders according to the invention may comprise any of the features set forth in the description, taken alone or in any technically possible combination with other characteristics.
  • the P powders considered are actinide powders making it possible to produce pellets of nuclear fuel.
  • the cryogenic fluid considered here is liquefied nitrogen.
  • the invention is not limited to these choices.
  • FIG. 1 With reference to the figure 1 , there is shown a diagram illustrating the general principle of a device 1 for mixing powders P by cryogenic fluid according to a first embodiment of the invention.
  • the device 1 comprises a number n of mixing chambers E1,..., In powders P, successively arranged in series one after the other in the same vertical direction so that the powders can circulate through mixing chambers E1, ..., under the effect of the force of gravity.
  • the device 1 comprises an n-1 number of passage restriction systems R1,..., Rn-1 of the powders P, each passage restriction system R1,..., Rn-1 being situated between two mixing chambers E1, ..., In successive, to constrain the distribution of powders P of a mixing chamber E1, ..., En to the following. Examples of such passage restriction systems R1,..., Rn-1 are presented hereinafter with particular reference to Figures 3 and 4 .
  • the device 1 also comprises two feed enclosures A1 and A2 in powders P, provided in particular for dispensing powders of different types.
  • the two feed enclosures A1 and A2 in powders P allow the introduction of powders P into the first mixing chamber E1 in contact with the cryogenic fluid FC of the first enclosure E1. Then, the powders P successively pass through the passage restriction systems R1,..., Rn-1 and the mixing chambers E2,..., In each mixing enclosure comprising a cryogenic fluid FC.
  • each mixing chamber E1,... Comprises stirring means 2 for mixing the powders P suspended in the cryogenic fluid FC.
  • stirring means 2 are given hereinafter with particular reference to Figures 3 and 4 .
  • the two feed enclosures A1 and A2 comprise for example adjustable feed hoppers, for example using a worm, and / or metering-type systems, including trays or vibrating corridors.
  • the device 1 further comprises an electrostatic charging system C +, C- powders P introduced into the mixing chambers E1, ..., En.
  • the part of the powders P contained in the first feed enclosure A1 is brought into contact with the positive part C + of the electrostatic charge system to be electrostatically charged in a positive manner, while the part of the powders P contained in the second A2 supply enclosure is brought into contact with the negative part C- of the electrostatic charge system to be electrostatically charged in a negative manner.
  • the device 1 comprises, in addition to the elements described above with reference to the figure 1 an agitating motor 5 capable of rotating first stirring means 2a in the form of mixing wheels 2a in the mixing chambers E1, ..., En.
  • These mixing mobiles 2a may comprise grinding mobiles. These mixing mobiles 2a can also comprise blades, quilt mobiles, turbines and / or blades, these types of mobiles being respectively represented on the blades. FIGS. 5A, 5B and 5C . In the exemplary embodiments of Figures 3 and 4 the mixing mobiles 2a comprise turbines.
  • the device 1 also comprises second stirring means 2b in the form of ultrasonic vibration generating means comprising sonotrodes 2b.
  • the passage restriction systems R1,..., Rn-1 comprise diaphragms.
  • the passage restriction systems R1,..., Rn-1 comprise sieves, more specifically sieve meshes.
  • the passage restriction systems R1,..., Rn-1 have an adjustable passage section and are thus arranged in such a way that their passage sections are classified from the largest to the thinnest in the direction downstream of the powders stream P.
  • the passage sections of these passage restriction systems R1,..., Rn-1 are smaller than the natural flow section of the powders P in order to force the deagglomeration before the passage through these sections.
  • Table 1 below thus gives the dimensioning obtained from a device 1 according to the invention for obtaining 1 kg / h of ground material.
  • Table 1 ⁇ i> ⁇ u> Table 1 ⁇ / u> ⁇ /i> Features of the device 1 Values Volume of a mixing chamber E1, ..., in 100 mL Diameter of a mixing chamber E1, ..., in 10 cm P powder content in the suspension 10% Rotation frequency of mixing mobiles 8 s -1 Diameter of a mixing mobile 4cm Pump flow 3.7.10 -4 m 3 / s Flow rate 7.5.10 -4 m 3 / s Mixing time (tm) for an enclosure with a 10% charge (A) ⁇ 0.40 s Mixing capacity ⁇ 0.9 kg / h Number of mixing chamber 4 Stirring power 105 W / m 3
  • the series of n mixing enclosures E1, ..., Having a unit volume Vn such that the overall volume V of mixing chambers E1, ..., En such that V n.Vn .
  • the overall mixing time is less than the mixing time tm for the volume V.
  • the difference is greater between these mixing times than n is large, as shown in the graph. of the figure 7 , representing the evolution X of the mixture as a function of time t, in a manner similar to the figure 6 , with the times t1 and t2 of the first and second speakers and the times t'm and tm.
  • FIG. 8 a diagram illustrating a device 1 for mixing powders P by cryogenic fluid according to a second embodiment of the invention.
  • the device 1 comprises a single mixing chamber E1 and mixing means MG of the mixing chamber E1 according to a gyroscopic movement.
  • these mixing means MG are in a gyroscopic type of movement, or close to being, allowing the rotation of the mixing chamber E1 along the three axes X1, X2 and X3 of the three-dimensional metrology.
  • This type of gyro-motion stirring favors the mixing of powders P when they have high densities compared to the density of the cryogenic fluid phase FC located in the mixing chamber E1.
  • the mixing chamber E1 comprises stirring means 2a, for example in the form of turbines.
  • Figures 9, 10 and 11 respectively represent photographs of a first type of powders before mixing, a second type of powders before mixing, and the mixture obtained of the first and second types of powders after mixing by means of a device 1 and a process according to the invention.
  • the figure 9 represents aggregates of cerium dioxide powders CeO 2
  • the figure 10 represents aggregates of alumina powders Al 2 O 3
  • the figure 11 represents the mixture of these powders obtained with a mixing time of about 30 s and the use of a single mixing chamber containing liquid nitrogen as a cryogenic mixing fluid.

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Claims (15)

  1. Vorrichtung (1) zum Mischen von Pulvern (P), insbesondere von Actinidpulvern, durch kryogenes Fluid, zumindest enthaltend:
    - eine Mehrzahl von Mischkammern (E1 - En) zum Mischen der Pulver (P), die jeweils ein kryogenes Fluid (FC) enthalten und aufeinanderfolgend in Reihe nacheinander angeordnet sind,
    - eine Zuführkammer (A1, A2) zum Zuführen von Pulvern (P), um das Einbringen von Pulvern (P) zumindest in die erste Mischkammer (E1) zu ermöglichen,
    - eine Mehrzahl von Systemen (R1 - Rn-1) zum Beschränken des Durchtritts von Pulvern (P), wobei jedes Durchtrittsbeschränkungssystem (R1 - Rn-1) zwischen zwei aufeinanderfolgenden Mischkammern (E1 - En) liegt, um die Ausgabe von Pulvern (P) von einer Mischkammer (E1 - En) zur nächsten zu begrenzen, wobei jedes Durchtrittsbeschränkungssystem (R1 - Rn-1) einstellbar ist,
    - Rühreinrichtungen (2, 2a, 2b) in jeder der Mischkammern (E1 - En), um das Mischen von in dem kryogenen Fluid (FC) in Suspension gebrachten Pulvern (P) zu ermöglichen.
  2. Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, dass das kryogene Fluid (FC) eine schwach hydrierte Flüssigkeit enthält, d.h. eine Flüssigkeit, die pro Flüssigkeitsmolekül höchstens ein Wasserstoffatom enthält und eine niedrigere Siedetemperatur als Wasser aufweist.
  3. Vorrichtung nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Rühreinrichtungen bewegliche Mischkörper (2a), insbesondere Schaufeln, Turbinen und/oder bewegliche Körper mit Deckwirkung, insbesondere bewegliche Mischkörper (2a) mit beweglichen Zerkleinerungseinrichtungen enthalten.
  4. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass die Rühreinrichtungen Einrichtungen zum Erzeugen von Schwingungen (2b), insbesondere Ultraschallschwingungen, insbesondere Sonotroden (2b), enthalten.
  5. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass die Durchtrittsbeschränkungssysteme (R1 - Rn-1) Siebe und/oder Membrane enthalten.
  6. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass die Durchtrittsbeschränkungssysteme (R1 - Rn-1) so ausgelegt sind, dass deren Durchtrittsquerschnitt in Abhängigkeit von dem Strömungsfluss der Pulver (P) durch die Mehrzahl von Mischkammern (E1 - En) hindurch abnimmt, wobei der Durchtrittsquerschnitt von einem (n-1)ten Durchtrittsbeschränkungssystem (Rn-1) somit größer ist als der Durchtrittsquerschnitt eines n-ten Durchtrittsbeschränkungssystems (Rn) in Richtung des Strömungsflusses der Pulver (P).
  7. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass der Durchtrittsquerschnitt der Durchtrittsbeschränkungssysteme (R1 - Rn1) kleiner ist als der eigentliche Strömungsquerschnitt der Pulver (P).
  8. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass die Mehrzahl von Mischkammern (E1 - En) und die Mehrzahl von Durchtrittsbeschränkungssystemen (R1 - Rn-1) für die Pulver (P) in einer gleichen vertikalen Richtung angeordnet sind, so dass ein Strömen der Pulver (P) unter der Wirkung von Schwerkraft möglich ist.
  9. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass sie ein System (C+, C-) zum elektrostatischen Aufladen von Pulvern (P) enthält, die in die Mischkammer bzw. Mischkammern (E1 - En) eingebracht werden sollen, wobei ein Teil der Pulver (P) insbesondere mit einem Teil des elektrostatischen Aufladesystems (C+) in Kontakt gebracht wird, um elektrostatisch positiv aufgeladen zu werden, und der andere Teil der Pulver (P) insbesondere mit dem anderen Teil des elektrostatischen Aufladesystems (C-) in Kontakt gebracht wird, um elektrostatisch negativ aufgeladen zu werden, um eine differenzierte lokale Agglomeration zu ermöglichen.
  10. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass das kryogene Fluid (FC) verflüssigter Stickstoff ist.
  11. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass sie zumindest zwei Zuführkammern (A1, A2) zum Zuführen von Pulvern (P) und insbesondere ebenso viele Zuführkammern (A1, A2) zum Zuführen von Pulvern (P) wie Arten von zu mischenden Pulvern (P) aufweist.
  12. Vorrichtung nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass die Zuführkammern (A1, A2) verstellbare Zuführtrichter und/oder Dosiersysteme, insbesondere Vibrationsplatten oder -rinnen, enthalten.
  13. Verfahren zum Mischen von Pulvern (P) durch kryogenes Fluid, das mittels einer Vorrichtung (1) nach einem der vorangehenden Ansprüche durchgeführt wird und die nachstehenden Schritte umfasst:
    a) Einbringen von zu mischenden Pulvern (P) in die Mischkammer bzw. Mischkammern (E1 - En) über die Zuführkammer bzw. Zuführkammern (A1, A2),
    b) Mischen der Pulver (P) in der Mischkammer bzw. den Mischkammern (E1 - En), welche Pulver in kryogenem Fluid (FC) in Suspension gebracht sind, über die Rühreinrichtungen (2, 2a, 2b)
    c) Gewinnen eines aus Pulvern (P) gebildeten Gemisches.
  14. Verfahren nach Anspruch 13, dadurch gekennzeichnet, dass im Laufe von dem ersten Schritt a) die Pulver elektrostatisch unterschiedlich, insbesondere gegensätzlich, geladen werden, um die differenzierte lokale Agglomeration zu begünstigen.
  15. Verfahren nach Anspruch 13 oder 14, dadurch gekennzeichnet, dass es ferner den Schritt des progressiven Beschränkens von dem Strömungsdurchtritt der Pulver (P) durch die Mischkammern (E1 - En) hindurch über die Durchtrittsbeschränkungssysteme (R1 - Rn-1) mit einem Durchtrittsquerschnitt, der in Richtung des Strömungsflusses der Pulver (P) abnimmt, umfasst.
EP16791565.1A 2015-11-04 2016-11-03 Vorrichtung zum mischen von pulvern mit kryogenem fluid und verfahren Active EP3370855B1 (de)

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FR1560570A FR3042985A1 (fr) 2015-11-04 2015-11-04 Dispositif de melange de poudres par fluide cryogenique
PCT/EP2016/076506 WO2017076944A1 (fr) 2015-11-04 2016-11-03 Dispositif de mélange de poudres par fluide cryogénique

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CN108348874B (zh) 2021-06-04
RU2018120089A3 (de) 2020-02-07
FR3042985A1 (fr) 2017-05-05
US10981126B2 (en) 2021-04-20
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