EP4452504B1 - Vorrichtung und verfahren zum berührungslosen mahlen und mischen von pulvern mit einem rotierenden innengehäuse - Google Patents

Vorrichtung und verfahren zum berührungslosen mahlen und mischen von pulvern mit einem rotierenden innengehäuse

Info

Publication number
EP4452504B1
EP4452504B1 EP22840254.1A EP22840254A EP4452504B1 EP 4452504 B1 EP4452504 B1 EP 4452504B1 EP 22840254 A EP22840254 A EP 22840254A EP 4452504 B1 EP4452504 B1 EP 4452504B1
Authority
EP
European Patent Office
Prior art keywords
grinding
mixing
inner casing
powders
tank
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP22840254.1A
Other languages
English (en)
French (fr)
Other versions
EP4452504C0 (de
EP4452504A1 (de
Inventor
Méryl BROTHIER
Stéphane VAUDEZ
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Original Assignee
Commissariat a lEnergie Atomique CEA
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Commissariat a lEnergie Atomique CEA, Commissariat a lEnergie Atomique et aux Energies Alternatives CEA filed Critical Commissariat a lEnergie Atomique CEA
Publication of EP4452504A1 publication Critical patent/EP4452504A1/de
Application granted granted Critical
Publication of EP4452504C0 publication Critical patent/EP4452504C0/de
Publication of EP4452504B1 publication Critical patent/EP4452504B1/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18—Details
    • B02C17/1815—Cooling or heating devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18—Details
    • B02C17/20—Disintegrating members
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18—Details
    • B02C17/24—Driving mechanisms

Definitions

  • the present invention relates to the field of powder grinding, in particular cryogenic grinding of powders, in particular in the liquid phase, to obtain submicron or even nanometric particles, while limiting impurities.
  • the invention preferably finds its application for any process and for any factory or industry implementing operations of mixing and/or grinding powders, in particular micronization of granular media with the aim in particular of obtaining improved performance in terms of specific energy applied and/or mixing or grinding time and/or in terms of grinding capacity of materials that are difficult to grind.
  • the invention thus proposes a device for grinding and mixing, preferably cryogenic, without contact of powders comprising an internal rotating protective casing located inside a grinding tank, as well as an associated grinding and mixing method, preferably cryogenic.
  • grinders are used that can vary greatly depending on the loads to be ground and their fragmentation capacity, such as knife, flail, hammer, roller, ball, air jet, and other mills.
  • CN112337587 describes a grinding device according to the preamble of the appended claim 1.
  • Known grinding devices suffer very largely, and recurrently, from pollution of the load by abrasion or wear induced by the grinding media and at the right of the grinding tank. This is due to the fact that the grinding media and/or the material to be ground have a hardness which may be greater than or equal to that of the material constituting the mill tank.
  • micronization of grinding powders is often complicated to optimize for targets with particle sizes below one micron and for materials known to be difficult to grind.
  • Micronization methods are inefficient, using speeds limited to a critical speed, which means that the materials have to be processed for several hours, or even several days, to achieve the desired particle sizes, thereby leading to pollution of the loads to be ground.
  • useful volume of micronizers is often small and submicron-targeted grinders are difficult or impossible to extrapolate to industrial scales.
  • a means is desired to efficiently apply energy to a powder in order to finely grind it, this powder being preferably suspended in a liquefied gas.
  • stirring energy allowing efficient operations to be carried out in terms of particle size or processing time, for example
  • the increase in stirring energy involves an increase in the speed of the mill's stirring rotor, there is concomitantly increased wear of the internals of the mill, at the right of which the differential speed of the wall/grinding balls and/or powder to be ground is the greatest.
  • the invention aims to at least partially remedy the needs mentioned above and the drawbacks relating to the achievements of the prior art.
  • the grinding and mixing device according to the invention may further comprise one or more of the following characteristics taken individually or in any possible technical combination.
  • the grinding and mixing device according to the invention is advantageously a cryogenic grinding and mixing device, the grinding tank comprising a cryogenic fluid, in particular liquid nitrogen, and being in particular heat-insulated, for example by means of an insulator of predetermined thickness.
  • the grinding tank is advantageously in the form of a reservoir providing thermal insulation, notably in the form of a double vacuum jacket, and allows the internal protective jacket to be received.
  • the grinding tank is advantageously made of a non-magnetizable material, for example stainless steel, in particular type 316L.
  • the internal volume of the internal protective envelope can advantageously include the grinding media.
  • the internal protective casing advantageously has a geometry similar to that of the grinding tank, being smaller in size so as to fit into the grinding tank.
  • the grinding and mixing unit can be driven in rotation by means of a drive system with a transmission arm.
  • the grinding and mixing unit can thus transmit the mechanical power delivered by the drive to the fluid to be ground in the form of convective movements by circular agitation.
  • Permanent magnets can be inserted into the inner protective casing or placed between the inner protective casing and the grinding tank.
  • the drive magnets may include fixed, non-rotating, reciprocating drive electromagnets located outside the grinding vessel.
  • the drive magnets may also include movable drive magnets, rotated by means of a drive motor.
  • the internal protective envelope may consist of or may include a coating in a material of hardness greater than that of the powders to be ground, in particular under cryogenic temperature conditions, and sublimating at room temperature and atmospheric pressure.
  • the inner protective envelope may in particular consist of or may include a coating of solidified carbon dioxide.
  • Carbon dioxide solidified can be obtained by solidification of liquid carbon dioxide by cooling or by compaction of dry ice or by machining.
  • the internal protective envelope may, for example, include raised attrition elements on its internal wall, in particular attrition pins, including solidified carbon dioxide.
  • the relief elements of attrition, or even grinding can be obtained by solidification of liquid carbon dioxide by cooling or by compaction of dry ice or by machining.
  • the permanent magnets and drive magnets can be arranged axisymmetrically with respect to the axis of rotation of the grinding tank.
  • Permanent magnets can be arranged by crimping and/or forcing.
  • the invention also relates, according to another of its aspects, to a method of grinding and mixing, in particular cryogenic grinding and mixing, of powders, characterized in that it is implemented by means of a device as defined above.
  • the method can advantageously be implemented by means of a cryogenic grinding and mixing device using a cryogenic fluid in the grinding tank, in particular liquid nitrogen, in direct contact with the powders to be ground.
  • the method may include the step of rotating the inner protective casing by means of fixed alternating drive electromagnets powered according to the distance between permanent magnets and electromagnets.
  • the method may further comprise the step of rotating the internal protective casing by means of mobile drive magnets rotated by means of a drive motor.
  • the rotation of the movable drive magnets can advantageously be carried out so that the direction of rotation varies alternately. In this way, it may be possible to increase the grinding efficiency.
  • the grinding and mixing device and method according to the invention may comprise any of the characteristics set out in the description, taken alone or in any technically possible combination with other characteristics.
  • FIG. 1 an example of a grinding and mixing device 1 according to the invention is shown with a first driving mode of the internal protective envelope.
  • the figure 2 represents the same grinding and mixing device 1 with a second mode of driving the internal protective casing.
  • the grinding and mixing device 1 is preferably a cryogenic grinding and mixing device. It advantageously allows the grinding and micronization of powders using a contactless drive wall so as to be able to limit the introduction of impurities, in particular by abrasion and wear of the internals of the grinding and mixing device.
  • the grinding and mixing device 1 firstly comprises a grinding tank 2.
  • the grinding tank 2 is in the form of a double jacket for maintaining a low partial pressure (at least primary vacuum) in the inter-wall volume formed by the double jacket. It thus ensures thermal insulation. It is advantageously made of a non-magnetizable material, for example stainless steel, in particular type 316L.
  • the grinding tank 2 has the function of receiving the load of solid powders P to be ground and mixed in liquid phase, in particular liquefied gas, for example liquid nitrogen.
  • the grinding tank 2 is generally cylindrical in shape. Its height is advantageously between 0.5 and 5 times its diameter. It may optionally include a low point drain that can be used to evacuate the load and/or recycle it within the tank 2.
  • the grinding tank 2 is designed to accommodate an internal protective casing 3 inserted between the grinding tank 2 and the fluid to be ground, powders and liquid.
  • the internal protective casing 3 comprises an internal volume Vi which may comprise grinding media Mb, for example balls, pellets, among others, visible on the Figures 1 and 2 . It advantageously has a geometry similar to that of the grinding tank 2, being of smaller size so as to fit into the grinding tank 2.
  • the inner protective envelope 3 consists mainly of solidified carbon dioxide CO 2 (s), i.e. CO 2 in a compact solid state, with a density at least equal to 60% of the theoretical density. This can be obtained by solidification of liquid carbon dioxide CO 2 (l) by cooling or by compaction of dry ice or by machining.
  • solidified carbon dioxide in contact with a liquefied gas at temperatures around -200°C at atmospheric pressure, solidified carbon dioxide becomes a relatively hard material since it goes from a hardness around 1.5 on the Mohs scale to a hardness close to 8 on the same scale.
  • the internal protective casing 3 comprises attrition pins 6 on its internal wall, which comprise solidified carbon dioxide CO 2 (s), obtained by solidification of liquid carbon dioxide CO 2 (l) by cooling or by compaction of dry ice or by machining.
  • the length of the attrition pins 6 is advantageously of an order of magnitude less than one sixth of the diameter of the grinding and mixing mobile 4.
  • the grinding and mixing device 1 comprises a grinding and mixing mobile 4 arranged in the internal volume Vi of the internal protective casing 3.
  • the grinding and mixing mobile 4 is driven in rotation by means of a motorization system with transmission arm.
  • the grinding and mixing mobile 4 can thus transmit the mechanical power delivered by the motorization to the fluid to be ground in the form of convective movements by circular movement agitation.
  • the motorization can advantageously comprise an electric motor equipped with a speed variator allowing it to be adjusted between a few tens of revolutions per minute, typically of the order of 50 revolutions/min, to a few thousand revolutions per minute, potentially up to 10,000 or even 20,000 revolutions/min.
  • the grinding and mixing mobile 4 can be of different types, for example of the turbine type, inclined or non-inclined blades, attrition mobile or propeller. It has a diameter of the grinding and mixing mobile such that the ratio between the diameter of the tank and the diameter of the grinding and mixing mobile is between 0.2 and 0.9.
  • the grinding and mixing device 1 comprises permanent magnets 7 located at the level of the internal protective casing 3. These permanent magnets 7 are inserted into the internal protective casing 3, as shown, or alternatively placed between the internal protective casing 3 and the grinding tank 2.
  • the grinding and mixing device 1 also comprises drive magnets 8a, 8b, for rotation, arrow R on the Figures 3 and 4 , of the internal protective casing 3 by interaction with the permanent magnets 7, located outside the grinding tank 2 opposite the permanent magnets 7.
  • the drive magnets 8a, 8b comprise fixed, non-rotationally driven, alternating drive electromagnets 8a placed outside the grinding tank 2.
  • the drive magnets 8a, 8b comprise movable drive magnets 8b, driven in rotation by means of a drive motor 9.
  • the permanent magnets 7 and the drive magnets 8a, 8b are arranged axisymmetrically with respect to the axis of rotation X of the grinding tank 2.
  • the permanent magnets 7 can be arranged by crimping and/or by forcing.
  • the grinding and mixing device 1 therefore allows both the use of an internal protective casing 3 based on solidified carbon dioxide (CO 2 (s)) but also the rotation of this casing 3 at angular speeds potentially equivalent to those of the grinding and mixing mobile 4.
  • CO 2 (s) solidified carbon dioxide
  • the inner protective casing 3 is rotated in the opposite direction to the rotation of the grinding and mixing mobile 4.
  • the rotation speed is less than or equal to the rotation speed of the grinding and mixing mobile 4.
  • the rotation of the internal protective casing 3 is ensured by means of the drive motor 9 and the moving magnets 8b or by means of the alternating electromagnets 8a.
  • Figures 3 and 4 illustrate the movement of the internal protective casing 3 by means of alternating electromagnets 8a.
  • the electromagnets 8a are powered from the moment when, at a given time t0 represented on the figure 3 , the distance between the permanent magnet 7 of the internal protective casing 3 and the electromagnet 8a becomes less than the maximum distance d max of magnetic influence, shown in the figure 3 . Then, from the moment, at time t1 represented on the figure 4 , where the two normals of the magnetic surfaces (surface of the permanent magnet 7 and surface of the electromagnet 7) form a limit angle ⁇ limit , visible on the figure 4 , tending towards zero, the power supply to the electromagnet 8a is interrupted.
  • Figures 5, 6 and 7 partially represent another example of a grinding and mixing device 1 according to the invention, using drive magnets in the form of electromagnets 8a.
  • the previously described references are not repeated here.
  • the permanent magnets 7 can be located between the internal protective casing 3 and the grinding tank 2.

Landscapes

  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Crushing And Grinding (AREA)

Claims (13)

  1. Mahl- und Mischvorrichtung (1) für Pulver (P), umfassend:
    - einen Mahlbehälter (2), umfassend die Beladung mit zu mahlenden Pulvern (P), insbesondere in der Flüssigphase, und Mahlmedien (Mb),
    - eine innere Schutzhülle (3), die im Inneren des Mahlbehälters (2) angeordnet ist und ein Innenvolumen definiert (Vi),
    - ein Mahl- und Mischmobil (4), das im Innenvolumen (Vi) der inneren Schutzhülle (3) angeordnet ist,
    dadurch gekennzeichnet, dass sie Folgendes umfasst:
    - Permanentmagnete (7), die sich an der inneren Schutzhülle (3) befinden,
    - Antriebsmagnete (8a, 8b) zum Drehen (R) der inneren Schutzhülle (3) durch Wechselwirkung mit den Permanentmagneten (7), die sich außerhalb des Mahlbehälters (2) gegenüber den Permanentmagneten (7) befinden.
  2. Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, dass es sich um eine kryogene Mahl- und Mischvorrichtung handelt, wobei der Mahlbehälter (2) ein kryogenes Fluid, insbesondere flüssigen Stickstoff (N2), aufweist und wärmeisoliert ist.
  3. Vorrichtung nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die innere Schutzhülle (3) aus einer Beschichtung aus einem Material, das eine Härte aufweist, die höher ist als die der zu mahlenden Pulver (P), insbesondere unter kryogenen Temperaturbedingungen, und das bei Umgebungstemperatur und atmosphärischem Druck sublimiert, besteht oder diese umfasst.
  4. Vorrichtung nach Anspruch 3, dadurch gekennzeichnet, dass die innere Schutzhülle (3) aus einer Beschichtung aus verfestigtem Kohlendioxid (CO2(s)) besteht oder diese aufweist.
  5. Vorrichtung nach Anspruch 4, dadurch gekennzeichnet, dass die innere Schutzhülle (3) an ihrer Innenwand erhabene Abriebelemente (6) aufweist, insbesondere Abriebstifte (6), die verfestigtes Kohlendioxid (CO2(s)) umfassen.
  6. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Permanentmagnete (7) in die innere Schutzhülle (3) eingesetzt oder zwischen der inneren Schutzhülle (3) und dem Mahlbehälter (2) platziert sind.
  7. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Antriebsmagnete (8a, 8b) feste, drehungsfreie Elektromagnete mit Wechselantrieb (8a) aufweisen, die außerhalb des Mahlbehälters (2) angeordnet sind.
  8. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Antriebsmagnete (8a, 8b) bewegliche Antriebsmagnete (8b) aufweisen, die über einen Antriebsmotor (9) drehbar angetrieben werden.
  9. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Permanentmagnete (7) und die Antriebsmagnete (8a, 8b) axialymmetrisch zur Drehachse (X) des Mahlbehälters (2) angeordnet sind.
  10. Mahl- und Mischverfahren für Pulver (P), dadurch gekennzeichnet, dass es mittels einer Vorrichtung nach einem der vorhergehenden Ansprüche durchgeführt wird.
  11. Mahl- und Mischverfahren nach Anspruch 10, dadurch gekennzeichnet, dass es mittels einer kryogenen Mahl- und Mischvorrichtung unter Verwendung eines kryogenen Fluids im Mahlbehälter (2), insbesondere flüssigen Stickstoff, in direktem Kontakt mit den zu mahlenden Pulvern (P) durchgeführt wird.
  12. Mahl- und Mischverfahren nach Anspruch 10 oder 11, dadurch gekennzeichnet, dass es den Schritt des Drehens der inneren Schutzhülle (3) durch bewegliche Antriebsmagnete (8b) umfasst, die über einen Antriebsmotor (9) in Drehung versetzt werden.
  13. Mahl- und Mischverfahren nach Anspruch 10 oder 11, dadurch gekennzeichnet, dass die Drehung der beweglichen Antriebsmagnete (8b) so erfolgt, dass die Drehrichtung abwechselnd variiert.
EP22840254.1A 2021-12-21 2022-12-05 Vorrichtung und verfahren zum berührungslosen mahlen und mischen von pulvern mit einem rotierenden innengehäuse Active EP4452504B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR2114145A FR3130647B1 (fr) 2021-12-21 2021-12-21 Dispositif et procédé de broyage et de mélange sans contact de poudres comportant une enveloppe interne tournante
PCT/FR2022/052251 WO2023118679A1 (fr) 2021-12-21 2022-12-05 Dispositif et procédé de broyage et de mélange sans contact de poudres comportant une enveloppe interne tournante

Publications (3)

Publication Number Publication Date
EP4452504A1 EP4452504A1 (de) 2024-10-30
EP4452504C0 EP4452504C0 (de) 2025-07-30
EP4452504B1 true EP4452504B1 (de) 2025-07-30

Family

ID=81328231

Family Applications (1)

Application Number Title Priority Date Filing Date
EP22840254.1A Active EP4452504B1 (de) 2021-12-21 2022-12-05 Vorrichtung und verfahren zum berührungslosen mahlen und mischen von pulvern mit einem rotierenden innengehäuse

Country Status (3)

Country Link
EP (1) EP4452504B1 (de)
FR (1) FR3130647B1 (de)
WO (1) WO2023118679A1 (de)

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6902699B2 (en) * 2002-10-02 2005-06-07 The Boeing Company Method for preparing cryomilled aluminum alloys and components extruded and forged therefrom
FR3072308B1 (fr) 2017-10-12 2019-11-15 Commissariat A L'energie Atomique Et Aux Energies Alternatives Dispositif et procede de broyage cryogenique avec media de broyage sous forme de gaz cryogenique solidifie
CN112337587B (zh) * 2020-11-20 2022-01-25 重庆市赛特刚玉有限公司 一种棕刚玉球磨机
CN112827584B (zh) * 2020-12-31 2024-11-26 生态环境部南京环境科学研究所 一种立式高温搅拌球磨设备
CN112827580B (zh) * 2020-12-31 2024-11-26 生态环境部南京环境科学研究所 一种高温行星球磨设备

Also Published As

Publication number Publication date
EP4452504C0 (de) 2025-07-30
WO2023118679A1 (fr) 2023-06-29
FR3130647A1 (fr) 2023-06-23
FR3130647B1 (fr) 2023-11-10
EP4452504A1 (de) 2024-10-30

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