EP3618966B1 - Broyeur tridimensionnel, son procédé de mise en oeuvre et ses utilisations - Google Patents

Broyeur tridimensionnel, son procédé de mise en oeuvre et ses utilisations Download PDF

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Publication number
EP3618966B1
EP3618966B1 EP19725763.7A EP19725763A EP3618966B1 EP 3618966 B1 EP3618966 B1 EP 3618966B1 EP 19725763 A EP19725763 A EP 19725763A EP 3618966 B1 EP3618966 B1 EP 3618966B1
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EP
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Prior art keywords
stationary
chamber
mill
milling chamber
heating device
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EP19725763.7A
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German (de)
English (en)
French (fr)
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EP3618966A1 (fr
Inventor
Julien THIEL
François Lacoste
Valentin LAIR
Samy HALLOUMI
Irène MALPARTIDA
Benoît MOEVUS
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Deasyl SA
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Deasyl SA
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Priority to PL19725763T priority Critical patent/PL3618966T3/pl
Publication of EP3618966A1 publication Critical patent/EP3618966A1/fr
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    • 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
    • B02C17/163—Stirring means
    • 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

Definitions

  • the present invention relates to the field of three-dimensional grinders capable of allowing micro-grinding of at least one raw material.
  • the present application relates to a three-dimensional crusher having within it a heating device, and in particular an induction heating device.
  • the invention relates to a process for using the aforementioned crusher, as well as to its uses, in particular in order to carry out synthetic reactions of organic or inorganic chemistry.
  • This grinder comprises in particular a cylindrical or conical grinding chamber, extending along a longitudinal axis, which serves to receive the microbeads and the liquid medium.
  • the chamber has at one end: a product inlet and at its other end, opposite the first, a product outlet.
  • the mill also comprises a mixer which is coaxial with the axis of the chamber and which is able to pivot so as to set the liquid medium and the microspheres in motion.
  • the mixer also has several mixing members distributed over its length in order to promote grinding.
  • This type of mill is used in particular in the pharmaceutical field in order to reduce the diameter of a product, for example of the order of a micrometer to a nanometer.
  • the FROM 44 34 940 describes a crusher intended to grind / crush an object, such as stone or the like and which comprises a casing comprising a cylindrical wall delimiting a grinding chamber, an agitator disposed in the chamber and which comprises a feed tube in which can circulate a hot medium or a cold medium in order to heat or cool the object during grinding.
  • the document KR 101 822 480 d wrote a process to produce organic fertilizer from organic waste from plants or animals.
  • This document describes in particular that the starting organic waste from plants or animals are mixed in a transfer mixer comprising a screw stirrer while being heated to a temperature ranging from 40 to 645 ° C, then they are pulverized in a grinder at a temperature ranging from 50 to 65 ° C.
  • the document DE 100 64 828 describes a mill comprising an annular heating or cooling chamber disposed at the periphery of a grinding chamber.
  • JP 2001 180933 and JP 2009 0006333 also describe a ball mill in order to grind an object.
  • the object of the present invention is thus to provide a novel three-dimensional mill capable in particular of improving the dispersion or the bringing into contact of at least one starting compound, preferably of at least two, which can be used industrially and which is simple to put into contact. artwork.
  • the heating device is an induction heating device.
  • the mill according to the invention makes it possible to carry out mechanical synthesis reactions, in particular continuously, which are effective via the presence of the heating device, such as an induction heating device.
  • the heating device such as an induction heating device.
  • the heating device makes it possible for example to activate chemical synthesis reactions.
  • organic or inorganic chemistry requiring a certain reaction temperature, to be able to use starting compounds which may be in liquid form depending on their melting point, or to use starting compounds whose viscosity is not suitable for ambient temperature.
  • the mill according to the invention is no longer intended for the starting compound in powder form, which is the general use of a three-dimensional microbead mill.
  • the mill according to the invention has the advantage of forming a reactor allowing the efficient synthesis of chemical compounds because it is capable of operating at temperature, and also of increasing the yields of these chemical syntheses, while reducing the processing times.
  • usual reaction As illustrated in the experimental part below, the reaction times generally pass from 3 to 13 hours to a time less than 1 hour, typically less than 1 minute (example, transesterification reaction of dimethyl carbonate depending on the conversion rate wish).
  • the heating device such as an induction heating device, allows the initial mixture to be heated in the form of a liquid stream, even if the latter has a high flow rate and without heat dissipation. outside the grinder.
  • the heating device located at the heart of the stationary chamber makes it possible to bring sufficient heat energy to the continuous flow, that is to say to the continuous flow of the starting compound (s) in the liquid medium passing through the chamber. stationary.
  • a simple heating of the periphery of the stationary chamber would result in an overall loss because part of this energy would have been dissipated outside the bowl, which is not the case with the heating device according to the invention.
  • the present invention has the advantage of allowing the positioning (at the entrance and / or in the middle of the stationary chamber, etc.) and the adjustment (desired temperature) of said at least one heating device, such as a induction heating device, depending on the desired reaction.
  • the method comprises the following additional step: (v) cooling the final product, so that the latter has a temperature less than or equal to 60 ° C, preferably less than or equal to 50 ° C and typically less than or equal to 30 ° C.
  • the present invention relates to the use of the three-dimensional mill as described above for carrying out synthetic reactions of organic and inorganic chemistry or for milling at least one starting compound.
  • starting compound is understood to mean all compounds which may be present in liquid, gas, solid (powder, etc.) form, the starting compound generally being a reagent making it possible to carry out a chemical synthesis reaction with another starting compound. and / or the liquid medium depending on the desired reaction.
  • liquid medium any liquid medium making it possible to improve the mixing of the starting compound (s) with the grinding bodies, such as microbeads; depending on the desired reaction, this starting medium can also correspond to one of the reactants in excess.
  • final product is understood to mean the product obtained at the outlet of the mill including in particular also the intermediate reaction products.
  • the Applicant has focused on the development of a new improved three-dimensional mill, suitable for use on an industrial scale.
  • the Applicant has developed a mill making it possible to carry out, most often in a single step, chemical synthesis reactions exhibiting a good to excellent conversion rate, in very short reaction times (generally in less than one step). (one hour and typically in less than 10 minutes) at temperatures greater than or equal to 60 ° C. and this with relatively low energy consumption.
  • the three-dimensional grinder 100 comprises at least one stationary grinding chamber 1 having a wall 7 of generally cylindrical shape which surrounds an interior 8.
  • the wall 7 extends along a longitudinal axis XX, preferably horizontal.
  • This stationary grinding chamber 1 is configured to receive and mix at least one starting compound, generally at least two, in a liquid medium, so as to form an initial mixture.
  • the chamber 100 can receive a single starting compound.
  • the chamber can receive at least two distinct starting compounds. Generally, at least two starting compounds will be introduced into the stationary grinding chamber 1.
  • this stationary grinding chamber 1 is also intended to be partially filled with at least grinding bodies 6, such as microbeads 6.
  • the stationary chamber 1 comprises, at a first end 2 (upstream), an inlet 4 which opens out within the stationary grinding chamber 1 and which serves to introduce the starting compound (s) and the liquid medium.
  • This inlet 4 can also be used to introduce the microspheres 6 before the use of the mill 100.
  • the size and the nature of the microbeads 6 depend on the desired synthesis reaction and can be adjusted accordingly.
  • the grinding chamber 100 comprises, at a second end 3 (downstream), an outlet 5 which leads to the outside and which is configured to discharge a final product formed in the stationary grinding chamber 1.
  • the outlet 5 generally comprises a separation means (not shown), such as a sieve or a grid, suitable for discharging only the final product and consequently for retaining the microspheres 6 when the mill 100 is in operation.
  • a separation means such as a sieve or a grid
  • the input 4 is generally connected to at least one pump, for example peristaltic (not shown).
  • This pump makes it possible to bring the starting compound (s) or even the initial mixture, if it has been prepared beforehand, inside the stationary grinding chamber 1 via the inlet 4.
  • the starting compound (s), or the initial mixture prepared beforehand can for example be contained in at least one container, such as a tank.
  • the pump also makes it possible, during the operation of the three-dimensional grinder 100, to supply the starting mixture at a certain rate which is adjustable, hereinafter called “flow rate”. This flow rate also forms a current in the stationary chamber 1 making it possible to drive the starting mixture from the inlet 4 to the outlet 5.
  • the three-dimensional mill 100 also comprises an agitator 10 which comprises an elongated rod 11 along the longitudinal axis XX and which extends mainly around the first end 2 to beyond the second end 3 of the stationary chamber 1.
  • an agitator 10 which comprises an elongated rod 11 along the longitudinal axis XX and which extends mainly around the first end 2 to beyond the second end 3 of the stationary chamber 1.
  • This elongated rod 11 advantageously extends coaxially with the aforementioned longitudinal axis XX.
  • This stirrer 10 is in particular capable of pivoting so as to set in motion, in addition to the start of the aforementioned passage, the whole grinding body 6 and initial mixture.
  • the agitator 10 is configured to rotate on itself, along the longitudinal axis XX, via an elongated rod 11 (or rotary shaft), to impart within the stationary chamber 1 a swirling movement to the initial mixture and thus perform intense mixing between this initial mixture and the microbeads 6 present in the chamber 1 along the internal surface of the wall 7 of this chamber 1.
  • the agitator 10 via its elongated rod 11 can have a speed of rotation greater than or equal to 100 revolutions per minute, advantageously greater than or equal to 1000 revolutions per minute (rev / min), preferably greater than or equal to 2000 revolutions per minute and typically greater than or equal to 2,500 revolutions per minute.
  • a speed of rotation greater than or equal to 100 revolutions per minute comprises the following values: 100; 150; 200; 250; 300; 350; 400; 450; 500; 550; 600; 650; 700; 750; 800; 850; 900, 950, 1000, etc., or any interval between these values
  • "a speed of rotation greater than or equal to 1000 revolutions per minute” includes the following values: 1000; 1100; 1200; 1300; 1400; 1500; 1600; 1700; 1800; 1900; 2000; 2100; 2200; 2300; 2400; 2500; 2600; 2700; 2800; 2900; 3000; 3100; 3200; 3300; 3400; 3500; 3600; 3700; 3800; 3900; 4000, 4500; 5000; 5500; 6000; etc., or any interval between these values.
  • the agitator 10 has a speed of rotation ranging from 1000 rpm to 5000 rpm, in particular from 1500 rpm to 4500 rpm, preferably from 2000 rpm to 4000 rpm and typically 2800 to 3200 rpm.
  • the agitator 10 like the internal surface of the internal wall 7 of the chamber 1, can have various possible configurations shown for example on the diagram. figure 3 .
  • the agitator 10 comprises, along its elongated rod 11, “rotating” mixing members 22, 26, arranged perpendicular to the latter.
  • a mixing member 22 (called “first mixing member”) can also correspond to a susceptor of the heating means 20 according to the invention and is thus different from the other mixing members 26 (called “first mixing member”). “Other mixing devices”).
  • This first mixing member 22, as well as the other mixing members 26, may correspond to the mixing members described in the document US 5,597,126 .
  • they can include at least two circular disks parallel to one another, configured to set in motion the grinding bodies 6 (microbeads).
  • the number of these mixing elements 22, 26 within the grinding chamber 1 can vary from 2 to 8, preferably from 2 to 5.
  • These mixing members 22, 26 make it possible, on the one hand, to improve the grinding of the initial suspension by further mixing the microbeads 6 and, on the other hand, to accelerate the reaction time.
  • the agitator 10 can also comprise, along its rod 11, one or more “rotary” mixing elements 22, 26 which are also able to cooperate with “fixed” fingers 28, arranged perpendicularly to the internal wall 7 of chamber 1.
  • a finger 28 is in particular in the form of a ring which extends perpendicularly from the wall 7.
  • the mixing elements 22, 26 and the fingers 28 are arranged in staggered rows, namely the mixing elements 22, 26 and the fingers 28 are arranged alternately in the chamber 1.
  • the fingers 28 thus form counter-fingers, each disposed between two mixing members 22, 26.
  • the thickness of the rod 11 is increased compared to the previous configuration ( figure 3a ) so that the periphery of the mixing members 22, 26 is close to the internal wall 7 and that of the fingers 28 is close to the periphery of the rod of the agitator 10.
  • the volume of the chamber is reduced compared to the previous configuration, consequently allowing better mixing between the initial suspension, the microbeads 6 and the internal wall 7 of the chamber 1.
  • the volume of the chamber 1 can be further reduced as illustrated in figure 3c .
  • the agitator 10 has an external diameter slightly smaller than the internal diameter of the chamber 1, thus forming an annular chamber 12 of small volume arranged between the external wall of the agitator 10 and the internal wall 7 of the chamber 1.
  • the microbeads (not shown) are placed in this annular chamber 12.
  • the starting suspension is introduced through the inlet 4 with a certain flow rate, which will then travel through the annular chamber 12 until it reaches output 5, while being stirred by microbeads 6.
  • the geometry of the grinding chamber 1 and of the agitator 10 can be adjusted by a person skilled in the art depending on the desired reaction, as well as the desired reaction time.
  • the grinding chamber 1 includes an accelerator to improve grinding of the initial mixture. Since this accelerator is known to those skilled in the art, it will not be detailed below.
  • the stationary chamber has a diameter of 75 mm to 300 mm for a length of 80 mm to 900 mm and a stirrer 10 has a size of 65 mm to 260 mm.
  • the volume of the grinding chamber can vary from 0.35 L to 600 L, preferably from 0.35 L to 400 L, and typically from 0.35 L to 62 L.
  • a volume of the stationary chamber 1 ranging from 0.35 L to 600 L comprises the following values: 0.35; 0.5; 0.8; 1; 2; 3; 4; 5; 6; 7; 8; 9; 10; 15; 20; 25; 30 ; 35; 40; 45; 50; 55; 60; 65; 70; 80; 85; 90; 100; 110; 120; 130; 140; 150; 160; 170; 180; 190; 200; 210; 220; 230; 240; 250; 260; 270; 280; 290; 300; 350; 400; 450; 500; 550; 600 etc., or any interval between these values.
  • the microspheres 6 housed in the grinding chamber 3 of the mill 1 during its operation are substantially spherical in shape and have an average diameter less than or equal to 5 mm, generally ranging from 0.05 mm to 4 mm, preferably from 0.2 to 3 mm, in particular from 0.3 to 2 mm, and typically of the order of 0.5 to 1 mm.
  • the diameter of the microbeads is less than or equal to 1 mm and is typically of the order of 0.05 mm to 1 mm.
  • microbeads exhibiting high hardness and relatively good abrasion resistance.
  • the microbeads 6 have a Vickers hardness measured according to standard EN ISO 6507-1 (2005) greater than or equal to 900 HV1, preferably ranging from 900 HV1 to 1600 HV1, typically ranging from 1000 to 1400 HV1 and in particular ranging from 110 to 1300 HV1.
  • a Vickers hardness greater than or equal to 900 HV1 comprises the following values: 900; 910; 920; 930; 940; 950; 960; 970; 980; 990; 1000; 1010; 1020; 1030; 1040; 1050; 1060; 1070; 1080; 1090; 1000; 1110; 1120; 1130; 1140; 1150; 1160; 1170; 1180; 1190; 1200; 1300; 1400; 1500; 1600; 1700; etc., or any interval between these values.
  • the microbeads according to the invention have a high real density.
  • the microbeads according to the invention have a real density greater than or equal to 2 g / cm 3 , in particular ranging from 2 to 15 g / cm 3 , preferably from 3 to 12 g / cm 3 , and typically from 4 at 10 g / cm 3 .
  • the microbeads according to the invention can be ceramic microbeads (zirconium oxide ZrO 2 , zirconium silicate ZrSiO 4 ); steel microbeads, tungsten carbide microbeads, glass microbeads or a combination thereof.
  • the microspheres are made of ceramic because they do not generate pollution by their wear.
  • the microspheres are made of zirconium oxide.
  • the zirconium oxide microspheres can be stabilized by another oxide, such as cerium oxide, yttrium and / or silicon oxide.
  • compositions are suitable for forming the microbeads according to the invention: ⁇ i> Table 1 ⁇ /i> Composition of microbeads Hardness HV1 Real density (g / cm 3 ) Maker Zirconium oxide microbeads stabilized by cerium oxide 1180 ⁇ 6.10 Saint-Gobain (Zirmil®Y Ceramic Beads) or EIP (Procerox® ZO Cer) - 80% of ZrO 2 - 20% of CeO Yttrium stabilized zirconium oxide microbeads 1250 ⁇ 5.95 EIP (Procerox® ZO (Y)) - 95% ZrO 2 - ⁇ 5% Al 2 O 3 - Remainder: Y 2 O 3 Zirconium oxide microbeads stabilized by yttrium and silicon: > 700 > 4.80 Saint-Gobain (ER120 Ceramic Beads) - 78% ZrO 2 , - 12% Si
  • microbeads 6 suitable for the invention are not made of glass or exclusively of glass.
  • microbeads 6 represent, by volume, relative to the total volume of the stationary chamber 2 from 50% to 85%, preferably from 55% to 70%.
  • a volume of 50 to 85% comprises the following values: 50; 55; 60; 65; 70; 75; 80; 85; etc., or any interval between these values.
  • the grinder 100 comprises at least one heating device, such as for example an induction heating device 20 which is illustrated in particular on the figures 1 and 2 .
  • the induction heating device (s) 20 are integrated inside the stationary grinding chamber 1 and make it possible to heat at least one zone of said stationary grinding chamber 1.
  • the induction heating device or devices 20 are located at the entrance to the chamber 1, that is to say around the first end 2 so as to be able to heat the flow of initial mixture as soon as it is introduced and consequently enable and / or activate chemical synthesis.
  • the induction heating device 20 is carried by at least part of said stirrer 10, allowing the rotary movement of the induction heating device 20 around the longitudinal axis XX.
  • This characteristic has the advantage of allowing better heating of the flow forming the initial mixture.
  • the inductor 21 is a coil or a solenoid having turns which surround a part of said rod 11 of the agitator 10, advantageously an upstream section located on the side of the first end 2 as shown in Figure figure 1 .
  • the inductor 21 is in particular able to generate a magnetic field which will allow the heating of the conductive materials in its environment, and in particular of the susceptor 22 to which it is coupled. Indeed, the susceptor, which conducts electricity, is able to capture the magnetic field emitted by the inductor.
  • the inductor 21 is made of multi-stranded Litz wire and is thus wound on the rod 11 of the crusher 100.
  • a cable from IDPArtner 300 strands Litz Cu 9.425 mm2 6x50x0.2mm is suitable for the invention.
  • the three-dimensional grinder 100 does not include the grinding members 22 or 26, the stirring of the initial mixture being carried out in the annular chamber 12 of small volume.
  • the induction heating device 20 is preferably placed at the inlet of the chamber 1, at the junction between the rod 11 and the stirrer 10 of larger diameter.
  • the inductor 21, such as a coil, can surround the rod 11;
  • the susceptor 22 may have the form of a disc perpendicular to the rod 11 which surrounds said coil.
  • the coil and susceptor assembly can be rotated by the rod 11.
  • the three-dimensional mill 100 comprises mixing members 22 or 26.
  • the susceptor 22 may correspond to the first mixing member implanted at the level of the first end 2, namely to the mixing member closest to the end 2 of the stationary grinding chamber 1.
  • This first mixing member 22 is thus made of a material which conducts electricity in order to be able to form the susceptor.
  • this first mixing member can be made of a resistive material of the carbon steel type in order to have maximum coupling with respect to the magnetic field emitted by the inductor.
  • the choice of this material is also indicated in that it preferably exhibits resistance to creep at high temperature, such as 800 ° C.
  • the first mixing member 22 can be made of Phyterm® 260 stainless steel equivalent to Kara ferric stainless steel from ArcelorMittal grade K44. This material can be heated up to 700 ° C which allows the liquid flow passing through it to go from room temperature to the desired temperature.
  • the other mixing members 26 which are different from the first mixing member 22, ie they are not necessarily electrically conductive, can in particular be made of chromium cast iron or ceramic of the zirconium oxide type.
  • this first mixing member 22 generally comprises a base secured to the rod 11 of the stirrer 10.
  • the inductor 21 is located at this base.
  • the induction heating device 20 is connected to an alternating electric current generator arranged outside said grinding chamber 1 by means of at least one current supply means 27 which is coaxial with the rod 11. of the agitator 10.
  • the generator can have a power ranging from 5 to 15 kW and preferably from 10 kW with a frequency varying for example from 17 to 200 kHz. It has a capacitance box that can be in parallel or in series.
  • an ID Partner serial generator reference IX3600 model PO8010 is suitable for producing the crusher according to the invention.
  • the current feed means 27 may for example correspond to copper strands, preferably a current feed strand to the coil and a current feed strand to the generator. These strands can be connected to the generator by means of a contactor 29.
  • This supply means can modify the center of gravity of the rod 11 of the agitator 10. It can however be balanced by compensating for it by the insertion. screws, for example in tungsten
  • the contactor 29 is also coaxial with the rod 11 of the agitator 10. This arrangement has the advantage of supplying the coil with current when the agitator 10 is rotating.
  • the generator supplies a sinusoidal alternating current, the frequency of which is defined by the oscillation of the system constituted by the assembly: generator capacity box, the inductor 21 and the current supply 27.
  • the generator current is then delivered to the inductor 21 by the contactor 29 connected to the latter via the current supply means 27.
  • the inductor 21, supplied with current will then be able to generate a magnetic field which will be picked up by the first mixing member 22 and allow it to be heated.
  • This first mixing member 22, which is rotated by the rod 11 of the agitator 10 will then be able to heat efficiently by thermal conduction the initial mixture (flow) passing through the grinding chamber 1.
  • the stationary grinding chamber 1 incorporates a magnetic screen 23 disposed between said inductor 21 and said rod 11 of the stirrer 10, so as to direct the heating towards the initial mixture.
  • the agitator 10 or its rod 11 is made of an electrically conductive material and thus, in order to avoid any overheating of the agitator 10, it is preferable to protect the agitator 10 or at least the rod part 11 which is surrounded by the inductor 21.
  • the magnetic screen 23 (with L-section) comprises a first tubular part 24 which is fitted over at least a part of the length of said rod 11 of the agitator 1, generally the part of the rod which is surrounded by the coil 21, and a second part in the form of a disc 25 or of a crown, connected to the first part 24, which is arranged in line with said rod 11.
  • This magnetic screen 23 also has the advantage of directing the magnetic field emitted by the coil 21 to the first mixing member 22 so that all the power is concentrated outside the inductor and in particular is not directed towards the rod. 11. Thus the heating zone is restricted to the outer periphery of the rod 11 and particularly concentrated on the first mixing member 22.
  • the magnetic screen can be a cylindrical torus made of Fluxtrol®.
  • the grinder 100 may include an induction heating device 20.
  • the crusher 100 comprises, as shown in figure 2 , two induction heaters 20.
  • the two heating devices 20 are generally assembled in series, namely a first heating device identical to the heating device described above is connected to a second heating device.
  • the second heater is also similar to the first heater, except that it is connected to the same generator and the same contactor as the first heater.
  • the current supply means of the second heating device is arranged between the first mixing member and the second mixing member, this second mixing member acting as a susceptor of the second heating means 20.
  • the latter is arranged in line with the rod 11 and comprises a base secured therewith.
  • the coil of the second heating means also surrounds the rod 11 at this base.
  • the second heating device also comprises a magnetic screen comprising two parts: a first tubular part which is fitted onto a part of the rod 11 going from the disk 25 of the magnetic screen of the first heating device to the coil of the second device. heating including the section surrounded by the coil, and a second part also in the form of a disc connected to the first part and which is arranged in line with the rod.
  • This second part makes it possible in particular to orient the magnetic field emitted by the coil towards the second mixing member.
  • the mill 100 may include more induction heaters 20. However, in general, one or two induction heaters 20 will suffice. to achieve the desired synthetic reactions.
  • the stationary grinding chamber 1 may include a pressure control means, such as at least one valve (not shown). It is thus possible to work in a controlled atmosphere.
  • the grinder 100 can include at least one temperature control means, such as one or more thermocouples placed on the surface of the grinding chamber 1. For example, they can be integrated at the inlet as well as 'at the outlet of the grinding chamber.
  • the crusher also comprises means 30 for cooling the final product, such as a heat exchanger, placed outside said stationary grinding chamber 1 on the side of the second end 3.
  • This cooling means 30 has the advantage of lowering the temperature of the final product so as to avoid possible thermal runaway.
  • the cooling means is suitable for lowering the temperature of the final product to a temperature which can reach room temperature (i.e. 15 and 30 ° C) or at least to a temperature making it possible to end the desired synthesis reaction.
  • the method comprises the following additional step: (v) cooling the final product, so that the latter has a temperature less than or equal to 60 ° C, preferably less than or equal to 50 ° C and typically less than or equal to 30 ° C.
  • the method according to the invention comprises step (i) comprising in particular starting up the heating device, such as the induction heating device 20.
  • the generator is put into operation in order to emit an alternating current which will be transmitted by the contactor and the current supply means to the coil 21.
  • the coil will then emit a variable magnetic field which will be. captured by the first mixing member 22.
  • This first mixing member 22, which is electrically conductive, will be immersed in this magnetic field thanks in particular to the magnetic screen which, on the one hand, protects the agitator 10 and of on the other hand directs the magnetic field towards it.
  • This will form at the level of this first mixing member an induced electric current, also called eddy current.
  • the movement of the electrons forming this induced current dissipates heat by the Joule effect at the level of the first mixing member.
  • the initial mixture is prepared, it is brought to the three-dimensional mill 100 by means, generally, of the peristaltic pump with adjustable flow rate via the inlet 4.
  • the peristaltic pump makes it possible to continue mixing the initial mixture before entry into chamber 1.
  • this pump makes it possible to introduce the starting suspension into chamber 1 with a controlled flow rate.
  • the initial mixture is introduced at a flow rate greater than or equal to 10 L / h.
  • a flow rate greater than or equal to 10 L / h comprises the following values: 10 L / h; 15 L / h; 20 L / h; 25 L / h; 30 L / h; 35 L / h; 40 L / h; 45 L / h; 55 L / h; 60 L / h; 65 L / h; 70 L / h; 80 L / h; 85 L / h; 90 L / h; 95 L / h; 100 L / h; 110 L / h; 120 L / h; 130 L / h; 140 L / h; 150 L / h; 50 L / h; 55 L / h; 60 L / h; 65 L / h; 70 L / h; 75 L / h; 80 L / h; 85 L / h; 90 L / h; 95 L / h; 100 L / h;
  • the initial mixture is introduced at a flow rate ranging from 10 to 130 L / h, preferably ranging from 20 to 100 L / h and typically ranging from 30 to 90 L / h.
  • the flow rates may vary depending on the size of the three-dimensional microbead mill used to carry out the process.
  • the flow rate may be of the order of 40 to 150L / h, such as approximately 45 L / h; while for larger mills having in particular a stationary chamber 2 of 60L, the flow rate may be of the order of 2 to 15 m 3 / h, such as approximately 4 m 3 / h.
  • the starting suspension travels through the stationary chamber 1 from the inlet 4 to the outlet 5, while being set in motion by the agitator 10 which allows an intense stirring of this suspension with the microbeads 6 and, where appropriate, with the mixing elements 26, the fingers 28, etc., along the internal wall 7 of the chamber 1.
  • the induction heating means 20 makes it possible to heat the flows passing through the chamber 1 to a temperature of at least 60 ° C, preferably ranging from 60 to 800 ° C, in particular from 60 to 400 ° C for a residence time less than or equal to 30 minutes, preferably less than or equal to 15 minutes, in particular less than or equal to 1 minute and in particular ranging from 5 to 25 seconds.
  • a temperature of at least 60 ° C.” comprises the following values: 60; 61; 62; 63; 64; 65; 66; 67; 68; 69; 70; 71; 72; 73; 75; 75; 80; 81; 82; 83; 84; 85; 86; 87; 88; 89; 90; 100; 110; 120; 130; 140; 150; 160; 170; 180; 190; 200; 210; 250; 300; 350; 400; 450; 500; 550; 600; 650; 700; 750; 800; 850; 900; 950; 1000; 1500; 2000; 2500; 3000; 3500; 4000; 4500; etc. and any intervals between these values.
  • a residence time less than or equal to 30 minutes comprises the following values: 30 min, 29 min, 28 min; 27 min; 26 min; 25 min; 20 min; 15 min; 14 min; 13 min; 12 min; 11 min; 10 minutes ; 9 min; 8 min; 7 min; 6 min; 5 minutes ; 4 min; 3 min; 2 min ; 1 min; 55 sec; 50 sec; 45 sec; 40 sec; 35 sec; 30 sec; 25 sec; 20 sec; 15 sec; 10 sec; 5 sec; etc. or any intervals between these values.
  • the residence time is generally inherent in the apparent volume of the beads and in the flow rate.
  • the residence time of the suspension in chamber 2 is estimated to be about 20 seconds. Consequently, the residence time can be advantageously adjusted, for example by controlling the bulk density of the microspheres, as well as the flow rate.
  • the term “apparent volume” is understood to mean the volume of the microbeads including the interstitial air between the beads.
  • the bulk density is the ratio of the mass of the microbeads to the apparent volume.
  • the speed of rotation of the agitator may for example vary from 4 to 20 Pi rad / s, preferably from 4 to 8 Pi rad / s.
  • the grinding step can be carried out in continuous mode or batch mode in one or more passes (pendulum mode or in recirculation).
  • the number of passages of the initial mixture and / or of the final product which is reintroduced into the grinding chamber can range from 1 to 50, preferably from 1 to 10, in particular from 1 to 5 (namely, after a first pass, the product obtained is recovered at outlet 5 and it is reinjected again, thanks to the pump, into chamber 1 via inlet 4 to allow a second pass).
  • a number of passages ranging from 1 to 50 comprises the following values: 50; 49; 48; 47; 45; 40; 35; 30 ; 25; 20; 15; 10; 9; 8; 7; 6; 5; 4; 3; 2; 1.
  • the number of passes of the starting suspension is 1 to 2, and preferably is 1.
  • this grinding step will preferably be carried out in continuous mode.
  • the final mixture is recovered (iv) at the outlet 5 of the grinder 100.
  • the final mixture is cooled by means of the heat exchanger.
  • This cooling makes it possible in particular to avoid, if necessary, a runaway of the chemical reaction carried out in the mill.
  • the cooling means is able to lower the temperature of the final product to a temperature which can reach room temperature (ie 15 and 30 ° C) or at least at a temperature making it possible to terminate the desired synthesis reaction.
  • the cooling of the final product is carried out so that it has a temperature less than or equal to 60 ° C, preferably less than or equal to 50 ° C and typically less than or equal to 30 ° C.
  • the final mixture is washed, dried and / or calcined.
  • the present invention also relates to the use of the three-dimensional mill 100 as described above for carrying out synthetic reactions of organic and inorganic chemistry or for milling at least one starting compound.
  • XRD X-ray diffractometry spectra
  • the detector used is an X'Celerator detector.
  • the DRX measurements were carried out between 5 ° and 70 ° (at the 2 ⁇ scale) with a step of 0.017 °.
  • the tests were carried out in a three-dimensional Dynomill ECM AP 2L microbead mill from the company Willy A. Bachofen AG, which contains 1 kg of microbeads, and which was adapted to include a heater 20 according to the invention as shown in figure 1 .
  • the mill includes a heater positioned at the entrance to the stationary chamber, and the first mixing member acts as a susceptor.
  • the heating device has the following characteristics: ⁇ i> Table 2 ⁇ /i> Elements Characteristics Generator 10kW power generator with a frequency varying from 17 to 200 kHz / IDPartner serial generator reference IX3600 model PO8010. Inductor Multistranded and resinated Litz threads to be removable. Cable from IDPartner 300 strands Litz Cu 9.425 mm 2 6x50x0.2mm. Susceptor Mixing device as described in the document US 5,597,126 ( fig.4 ) in Phyterm® 260 stainless steel equivalent to Kara ferric stainless steel from ArcelorMittal grade K44. Magnetic screen Cylindrical toroid in Fluxtrol® Current supply means The rod 11 has been modified to integrate the 3mm 2 coaxial copper current lead. This coaxial cable changes the center of gravity of the rod; it is thus balanced by compensating for it by the insertion of tungsten screws. Thermocouples Type K at the inlet and outlet of the grinding chamber. Contactor Copper rotary contactor.
  • the microspheres are made of zirconium oxide and have a diameter of 0.45 / 0.55 mm.
  • the characteristics of the microbeads used for the tests are summarized in Table 3 below: ⁇ i> Table 3 ⁇ /i> Balls 0.45 / 0.55 mm Composition (% by mass) 93% ZrO 2 5% Y2O3 2% other Specific density 6.0 g / cc Apparent volumetric mass 3.7 kg / l Vickers hardness 1250 HV1
  • the 0.45 / 0.55mm microbeads are in particular marketed under the brand name Zirmil® Y Ceramic Beads by the company Saint-Gobain.
  • the grinding chamber of the mill has a capacity of 2000 ml and is filled, by volume, relative to its total volume and depending on the tests, with 80% of the microbeads described above.
  • the microspheres are stirred by a stirrer at a speed of rotation of 2890 figures / min.
  • the agitator also features chrome cast iron mixing discs.
  • the starting raw materials are: zinc oxide (ZnO) having a purity of 99% marketed by the company Ampère Industries, and glycerol of purity 99.5%, marketed by the company Reactolab.
  • a comparative test was also carried out. This test was carried out using a process for manufacturing zinc glycerolate according to the prior art. This test consists of heating in a Z-shaped hand mixer capable of being heated (2L) zinc hydrozincite (1692 gr) with glycerol (428 gr), a Solsperse 21000 wetting agent (38 gr) and acetic acid as catalyst (3.6 g) for 4-5 hours at 120-130 ° C (example 1 from document US 7,074,949 ).
  • the mill according to the invention makes it possible to carry out the desired chemical synthesis reaction in very short residence times.
  • Example 2 carried out with the same catalyst as that described in the prior art and with a residence time of 20 seconds against 4-5 hours for the prior art, the yield obtained is 38%, against 10% without the use of a heating device according to the invention.
  • the yield of 38% could be improved by increasing the residence time of the initial mixture, for example with several passes in the stationary chamber or with a residence time of 1 to 2 minutes, still much less than 4-5 hours of the prior art.
  • Example 4 carried out with a catalyst different from that described in the prior art and with a residence time of only 20 seconds, a yield of 100% is obtained against 4 to 5 hours of the prior art, figure 4 .
  • the efficiency is 100% with the heating device against only 50% without it: the residual presence of the ZnO reagent is indeed observed on the diffractrogram, figure 4 .

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Crushing And Grinding (AREA)
  • Crushing And Pulverization Processes (AREA)
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JP7461303B2 (ja) 2024-04-03
JP2021528228A (ja) 2021-10-21
US20210213459A1 (en) 2021-07-15
CN112512694A (zh) 2021-03-16
FR3081732B1 (fr) 2020-09-11
EP3618966A1 (fr) 2020-03-11
ES2827282T3 (es) 2021-05-20
PL3618966T3 (pl) 2021-01-25
US11969734B2 (en) 2024-04-30
CN112512694B (zh) 2022-12-06
DK3618966T3 (da) 2020-10-26
KR102661290B1 (ko) 2024-04-30
WO2019228983A1 (fr) 2019-12-05
KR20210013568A (ko) 2021-02-04
FR3081732A1 (fr) 2019-12-06

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