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    • 专利摘要:
    The invention relates to a device for producing a dispersion comprising elements comprising a first phase, dispersed in a continuous phase immiscible with the first phase. The device comprises at least one production nozzle comprising: a first conduit intended to convey a first fluid forming the first phase; a second conduit coaxially surrounding a portion of the first conduit capable of conveying a second fluid forming the continuous phase; and - an exit. The nozzle is adapted to form at the outlet a fluid jet comprising the first fluid and the second fluid surrounding the first fluid. The production device further comprises a device for mechanical fragmentation of the fluid jet disposed in the vicinity of the outlet of the nozzle, the fragmentation device comprising a mobile part for mechanically breaking the fluid jet into a plurality of elements.
    公开号:FR3077011A1
    申请号:FR1850550
    申请日:2018-01-24
    公开日:2019-07-26
    发明作者:Yan Eric Pafumi；Mathieu Goutayer
    申请人:Capsum SAS；
    IPC主号:
    专利说明:

    Device for producing a dispersion, assembly and associated method
    The present invention relates to a device for producing a dispersion. The invention also relates to a production assembly comprising at least one such device as well as to a process for producing a dispersion using such a device.
    The Applicant manufactures and markets macroscopic dispersions comprising elements visible to the naked eye, for example with a diameter between 100 μm and 1500 μm, kinetically stable and optionally monodispersed.
    The production of a dispersion comprising elements dispersed in a continuous phase, for example of macro-emulsions, generally consists in mixing between at least two phases which are substantially immiscible with each other, either directly in the manufacturing tank or in a reactor. online.
    However, such methods make it very difficult, if not impossible, to obtain a homogeneous distribution of the elements dispersed in the continuous phase. It is also difficult to obtain high dispersed phase concentrations, as well as to obtain macroscopic dispersed elements, in particular of millimeter or greater size. These difficulties are further increased when one of the phases has a high viscosity, or when it is desired to obtain a high production rate.
    It is known to produce the elements of the dispersion in milli- or microfluidic devices, such as for example that described in WO2012 / 120043, in order to precisely control their dimensions and the homogeneity of their distribution in the continuous phase.
    These devices can be further improved. Indeed, they do not easily make it possible to obtain high production rates due to their hydrodynamic functioning, the separation of the elements according to a drip-type process (or English drippingen).
    These devices also impose limits in terms of viscosity or at least adaptations in terms of raw materials and / or devices, the fluids indeed having to be able to flow in channels of very small section. These drawbacks de facto limit the dosage and / or the sensoriality of the dispersions capable of being obtained and / or complicate the dispersion production process.
    An object of the invention is to provide a production device making it possible to easily obtain, with high production yields, dispersed elements, in particular macroscopic and if necessary monodisperse, and / or in high concentration, even in the presence of at minus a high viscosity phase, while easily mastering the effects of the change in production scale.
    Thus, the invention relates to a production device of the aforementioned type, characterized in that the dispersion comprising elements comprising at least a first phase, dispersed in a continuous phase substantially immiscible with the first phase, the device comprising:
    - At least one production nozzle comprising at least a first conduit intended to convey a first fluid suitable for constituting the first phase, a second conduit surrounding, preferably coaxially, at least a part of the first conduit, the second conduit being clean conveying a second fluid capable of constituting the continuous phase, and an outlet, the nozzle being adapted to form at the outlet a fluid jet comprising at least the first fluid and the second fluid surrounding the first fluid, preferably coaxially, and
    - At least one device for mechanical fragmentation of the fluid jet, arranged in the vicinity of the outlet of the nozzle, the fragmentation device comprising a part movable relative to the nozzle, intended to mechanically fragment the fluid jet into a plurality of elements comprising the first fluid dispersed in the continuous phase.
    According to particular embodiments, the device according to the invention has one or more of the following characteristics, taken separately or in any technically possible combination:
    - The mechanical fragmentation device is movable opposite the nozzle;
    the production nozzle comprises a third conduit, at least part of which is surrounded, preferably coaxially, by at least part of the first conduit, the third conduit being suitable for conveying a third fluid substantially immiscible with the first fluid, the fluid jet comprising the third fluid, the first fluid surrounding the third fluid, preferably coaxially, and the second fluid surrounding the first fluid, preferably coaxially, each element dispersed in the continuous phase comprising an external core formed by the first fluid, and at least one, preferably a single, inner core formed by the third fluid disposed in the outer core;
    - Each element comprises a bark, preferably formed of a layer of coacervate, at the interface between the first phase and the continuous phase, and optionally also at the interface between the first phase and the third fluid;
    the first phase of the elements forms a shell formed of a layer comprising at least one gelling agent, in particular chosen from a heat-sensitive gelling agent which is solid at room temperature and atmospheric pressure, a polysaccharide, in particular a polyelectrolyte reactive with multivalent ions, between the third fluid and the continuous phase;
    - The device comprises at least one independent conduit intended to convey to the dispersion an additional fluid comprising at least one solution for increasing the viscosity of the continuous phase;
    - The device comprises at least one heating device capable of heating at least the first fluid, and optionally the second fluid and / or the third fluid, at least in the production nozzle;
    - the mobile part of the fragmentation device comprises a rotary or oscillating scraper, provided with successive openings;
    - The successive openings are adapted to pass successively opposite the nozzle during the movement of the movable part relative to the nozzle;
    - The elements have a substantially spherical shape;
    - at least 60%, or even at least 70%, preferably at least 80%, and better still at least 90% of the elements have an average diameter greater than or equal to 10 μm, preferably greater than or equal to 50 μm, in particular greater or equal to 100 μm, or even greater than or equal to 200 μm, better still greater than or equal to 300 μm, and in particular greater than or equal to 400 μm; and
    the device further comprises at least one mixer capable of exerting on the elements a homogeneous controlled shear, said mixer comprising at least one cell formed by at least:
    - two coaxial rotary cylinders;
    - two parallel rotating discs; or
    - two parallel oscillating plates.
    According to a particular embodiment, in order to improve the monodispersity of the elements, the elements are subjected to a size refining step during which they are subjected to a shear capable of fragmenting them into elements of homogeneous and controlled diameters. Preferably, the refining step is carried out in a high shear cell of the Couette type, according to a process described in document EP3144058.
    The invention also relates to an assembly for producing a dispersion comprising a plurality of production devices as described above, and a fluid distribution system capable of supplying each device at least with first fluid and with second fluid and, optionally , as a third fluid, preferably the outlets of the nozzles opening into the same chamber.
    According to particular embodiments, the assembly according to the invention has one or more of the following characteristics, taken separately or in any technically possible combination:
    - The devices are arranged in at least one centripetal circle, the outputs of the nozzles being oriented towards a center of the circle;
    - the fragmentation device is common to all the devices; and
    - The mobile part of the common fragmentation device includes a rotary or oscillating scraper arranged to travel an internal contour of the centripetal circle.
    The invention further relates to a method of manufacturing a dispersion comprising elements comprising at least a first phase dispersed in a continuous phase, the method comprising at least the following steps:
    - Supply of a production device as described above and of at least a first fluid and a second fluid substantially immiscible with the first fluid;
    - flows of the first fluid in the first conduit, the first fluid forming the first phase and of the second fluid in the second conduit surrounding, preferably coaxially, the first conduit;
    - formation of a fluid jet at the outlet of the nozzle, the fluid jet, formed by co-extrusion, comprising at least the first fluid and the second fluid surrounding the first fluid, preferably coaxially;
    displacement of the mobile part of the fragmentation device to fragment the fluid jet and obtain elements comprising at least the first fluid dispersed in the second fluid; and
    - recovery of the dispersion.
    According to particular embodiments, the method according to the invention has one or more of the following characteristics, taken separately or in any technically possible combination:
    the method comprises a step of flowing a third fluid in a third conduit, at least part of the third conduit being surrounded, preferably coaxially, by at least a part of the first conduit, the fluid jet also comprising the third fluid, the first fluid surrounding the third fluid, preferably coaxially; and
    the method comprises a step of refining in size, during which a controlled and homogeneous shearing is applied to the elements in a mixer, the mixer being in particular of the Duvet type, comprising two coaxial cylinders, an external cylinder of internal radius R o and an internal cylinder of external radius R ,, the external cylinder being fixed and the internal cylinder being in rotation with an angular speed ω.
    According to a particular embodiment, the phases of the dispersion form a macroscopically inhomogeneous mixture. This is particularly the case when the dispersed elements have a macroscopic character.
    In the context of the present invention, the above-mentioned dispersions can be designated either by the term emulsions.
    According to one embodiment, the dispersions according to the invention do not comprise a surfactant.
    Finally, the invention relates to a composition, in particular a cosmetic composition, comprising at least one dispersion as described above and, optionally, a physiologically acceptable medium.
    The invention will be better understood on reading the description which follows, given solely by way of example and made with reference to the appended drawings, among which:
    - Figure 1 is a schematic view in longitudinal section of a production device according to the invention;
    - Figure 2 is a schematic view in longitudinal section of a second production device according to the invention;
    - Figure 3 is a perspective view of a production assembly according to the invention comprising a plurality of production devices;
    - Figure 4 is a view similar to Figure 1 of a production device according to the invention;
    - Figure 5 is a view of an example of dispersion according to the invention where the elements of the dispersion are in the form of drops formed by a device according to the invention;
    - Figure 6 is a view of an example of a dispersion according to the invention where the elements of the dispersion are in the form of capsules formed by a device according to the invention.
    Temperature and pressure
    Unless otherwise indicated, in all that follows, we consider that we are at ambient temperature (for example T = 25 ° C ± 2 ° C) and atmospheric pressure (760 mm Hg, i.e. 1,013,105 Pa or 1,013 mbar) .
    Viscosity
    The viscosity of the dispersions according to the invention can vary significantly, which makes it possible to obtain various textures.
    According to one embodiment, each of the phases forming a dispersion according to the invention and / or the dispersion according to the invention has a viscosity ranging from 1 mPa.s to 500,000 mPa.s, preferably from 10 mPa.s to 300 000 mPa.s, better from 400 mPa.s to 200,000 mPa.s, and more particularly from 2,000 mPa.s to 150,000 mPa.s, as measured at 25 ° C.
    The viscosity is measured at ambient temperature and at ambient pressure, by the method described in WO2016 / 096995.
    Referring to FIG. 1, a device 10 for producing a dispersion 12 according to a first embodiment of the invention is described, the dispersion 12 comprising elements 14 comprising a first phase 16, dispersed in a continuous phase 18.
    Dispersion 12
    The dispersion 12 is direct (i.e. of the oil-in-water type) or inverse (i.e. of the water-in-oil type). The dispersion 12 obtained is kinetically stable. By “kinetically stable”, within the meaning of the present invention, is meant for example that the dispersion is stable for at least two weeks, or even a month, preferably three months, and better still six months. By "stable" is meant that the dispersion retains a satisfactory visual homogeneity, that is to say without phase shift or creaming perceptible to the eye.
    The first phase 16 is aqueous or oily, preferably oily, and immiscible with the continuous phase 18 at room temperature and at atmospheric pressure.
    The continuous phase 18 is oily or aqueous, preferably aqueous, and in particular of a different nature from the first phase 16.
    As oils which can be used in the present invention, mention may be made of those described in the patent application filed under the number FR1759183.
    The elements 14 are advantageously substantially spherical and preferably macroscopic.
    Preferably, at least 60%, or even at least 70%, preferably at least 80%, and better still at least 90%, of the elements 14 have an average diameter D greater than or equal to 10 μm, preferably greater than or equal to 50 pm, in particular greater than or equal to 100 pm, or even greater than or equal to 200 pm, and better still greater than or equal to 300 pm, in particular greater than or equal to 400 pm. In particular, at least 60%, or even at least 70%, preferably at least 80%, and better still at least 90%, of the elements 14 have an average diameter D of between 10 μm and 3000 μm, in particular between 50 μm and 2500 pm, preferably between 100 pm and 2000 pm, in particular between 200 pm and 1500 pm, or even between 500 pm and 1000 pm.
    The elements 14 advantageously have an apparent monodispersity (that is to say that they are perceived to the eye as identical spheres in diameter).
    By “apparent monodispersity” is meant, for a given population of elements 14, a coefficient of variation Cv of the mean diameter D of the elements 14 between 10% and 30%, and better still between 15% and 20%.
    The average diameter D of the elements 14 is for example measured by analysis of a photograph of a batch consisting of N elements 14, by image processing software. Typically, according to this method, the diameter is measured in pixels, then reported in pm, depending on the size of the container containing the elements 14 of the dispersion 12.
    Preferably, the value of N is chosen to be greater than or equal to 30, so that this analysis statistically significantly reflects the distribution of diameters of the elements of said emulsion.
    The diameter Di of each element 14 is measured, then the average diameter D is obtained by calculating the arithmetic mean of these values:
    _ 1 N d = —Σ ° ί
    From these values Di, one can also obtain the standard deviation σ of the diameters of the elements 14 of the dispersion 12:
    The standard deviation σ of a dispersion reflects the distribution of the diameters Di of the elements of the dispersion 12 around the mean diameter D.
    By knowing the mean diameter D e t the standard deviation σ of a Gaussian dispersion, we can determine that we find 95.4% of the population of elements 14 in the range of diameters | p - 2σ, D + 2σ] and g ue ρ οη finds 58.2% of the population in the interval ÎP - D + σ]
    To characterize the monodispersity of the dispersion 12 according to this mode of the invention, the coefficient of variation can be calculated:
    This parameter reflects the distribution of the diameters of the elements 14 as a function of the average diameter of these.
    The coefficient of variation Cv of the diameters of the elements 14 is advantageously less than 30%, preferably less than 20%, and better still less than 10%, or even less than 5%.
    Alternatively, the monodispersity can be demonstrated by placing a sample of a dispersion according to the invention in a bottle with a constant circular section. A gentle agitation by rotation of a quarter of a turn for half a second around the axis of symmetry crossing the flask, followed by a rest of half a second is carried out, before repeating the operation in reverse, and this four times in a row.
    The elements of the dispersed phase are organized in a crystalline form when they are monodispersed. Thus, they have a stack in a pattern repeating in three dimensions. It is then possible to observe, a regular stacking which indicates a good monodispersity, an irregular stacking translating the polydispersity of the dispersion 12. If necessary, the skilled person will be able to adjust the viscosity of the phases, in particular of the continuous phase 18, for a satisfactory implementation of this method of characterizing monodispersity.
    The dispersion 12 can advantageously comprise a fraction greater than or equal to 2%, preferably greater than or equal to 5%, better still greater than or equal to 10%, in particular greater than or equal to 15%, better still greater than or equal to 20%, and in particular greater than or equal to 30% by weight of first phase 16, in particular of oil (s), relative to the total weight of the dispersion 12. On the contrary, with a drip process of the prior art, the maximum fraction achievable in oil (s) in direct dispersion is approximately 15%.
    Thus, the dispersion 12 can advantageously comprise a fraction of between 15% and 60%, preferably between 20% and 50%, in particular between 30% and 40%, by weight of first phase 16, in particular of oil (s ), relative to the total weight of the dispersion 12.
    In the embodiment shown in FIG. 1, each element 14 of the dispersion is formed from a drop of first phase 16.
    According to an alternative embodiment, each element 14 of the dispersion may comprise at least one bark 16A. A person skilled in the art will know how to make the adaptations and / or adjustments necessary to ensure the formation of this bark 16A, taking into account, in particular, the characteristics of the device according to the invention.
    For example, the bark 16A can be formed of a layer of coacervate at the interface between the first phase 16 and the continuous phase 18. This layer of coacervate is advantageously formed by interaction between at least one first precursor polymer of the coacervate initially. contained in the first phase 16 and at least one second precursor polymer of the coacervate initially contained in the continuous phase
    18. Thus, the first polymer is a hydrophilic polymer and the second precursor polymer is a lipophilic polymer, or vice versa. A pair "first coacervate precursor polymer / second coacervate precursor polymer" is in particular a "carbomer / amodimethicone" pair. Examples of elements of this type are described in WO2012120043.
    A device according to the invention is also advantageous in that it makes it possible to form a dispersion 12 by dispensing with the use of an intermediate liquid generally used to retard the migration of one of the two polymers involved. in the coacervation reaction towards the interface between the dispersed phase 16 and the continuous phase 18 and this, without fouling of the nozzle.
    According to a second variant (not shown), each element 14 of the dispersion 12 comprises at least a first gelling agent in the first phase 16 and optionally at least a second gelling agent in the continuous phase 18. In other words, the elements 14 of the dispersion 12 according to this second variant has improved kinetic stability and mechanical strength despite the absence of bark. The first phase 16 and / or the continuous phase 18 are for example gelled. Examples of hydrophilic or lipophilic gelling agents are described in the application filed under the number FR1752208.
    According to a third alternative embodiment (not shown), the dispersion 12 comprises at least a first gelling agent in the first phase 16 and optionally at least a second gelling agent in the continuous phase 18, each element 14 further comprising a shell, in particular formed of a coacervate layer at the interface between the first phase 16 and the continuous phase 18 by interaction between at least one first polymer initially contained in the first phase 16 and at least one second polymer initially contained in the continuous phase 18 This variant is advantageous in that it leads to further improved kinetic stability of the dispersion 12.
    Production device 10
    The device 10 comprises a production nozzle 20 capable of forming a fluid jet 22, a mechanical fragmentation device 24 intended to mechanically fragment the fluid jet 22 and a chamber 26 intended to contain and evacuate the dispersion 12.
    The nozzle 20 comprises at least a first conduit 30, a second conduit 32 and an outlet 34, defined in a frame 35 carrying the nozzle 20.
    The first conduit 30 and the second conduit 32 each comprise a succession of at least one substantially cylindrical conduit segment in the frame 35.
    The first conduit 30 is intended to convey a first fluid 36, suitable for forming the first phase 16, from a first channel 38 for supplying the first fluid 36. The first conduit 30 opens into the second conduit 32, for example halfway of the length of the second conduit 32. The segment of the first conduit 30 opening into the second conduit extends along a flow axis XX ′.
    According to a particular embodiment (not shown), the second conduit 32 and the first conduit 30 lead to the outlet 34 of the nozzle 20 on the same plane.
    The second conduit 32 is intended to convey a second fluid 40, capable of forming the continuous phase 18, from a second channel 42 for supplying the second fluid 40. The second conduit 32 opens at the outlet 34 of the nozzle 20, and surrounds , preferably coaxially, part of the first conduit 30 over part of the length of the second conduit 32.
    The segment of the second conduit 32 leading to the outlet 34 extends along the flow axis X-X ’.
    The nozzle 20 is thus able to form the fluid jet 22 by coextrusion at the outlet 34, the second fluid 40 surrounding, preferably coaxially, the first fluid 36 in the fluid jet 22. The fluid jet 22 flows in the vicinity of the outlet 34 in a direction substantially parallel to the flow axis XX ′.
    A person skilled in the art will know how to make the necessary adjustments, in particular at the level of the first fluid 36 and second fluid 40 flow rates to ensure the formation of the fluid jet at the outlet 34 of the nozzle 20.
    The outlet 34 is an opening in the frame 35, opening into the chamber 26. The opening 34 is part of an opening plane substantially orthogonal to the flow axis X-X ’.
    The mechanical fragmentation device 24 is arranged in the vicinity of the outlet 34 of the nozzle 20, and comprises a movable part 50 relative to the nozzle 34 and an actuator (not shown) intended to set in motion the movable part 50.
    The movable part 50 is capable of dividing the fluid jet 22 mechanically, that is to say that the movement of the movable part 50 cuts the fluid jet 22 regularly to divide it mechanically. The fractionation of the fluid jet 22 takes place at one time, and over a very short period, which makes it possible to control the mechanical action of fragmentation and the size of the elements 14.
    The movable part 50 has through openings 52 along the flow axis X-X ’, advantageously regularly spaced from each other. For example, the movable part 50 has the shape of a flat or cylindrical grid, comprising alternating bars or wires, in particular of metal, and openings 52.
    Each opening 52 advantageously has a transverse extent substantially equal to a transverse extent of the opening 34, in a plane orthogonal to the flow axis X-X ’. Thus, the opening 52 is adapted to allow the flow of the fluid jet 22 when it is opposite the outlet 34.
    The actuator is intended to set in motion the movable part 50 in a direction substantially transverse to the direction of flow of the fluid jet 22 through the outlet 34. The actuator comprises for example an electric motor and a rod-crank system.
    The mobile part 50 is thus mobile at least between a closed position, in which the outlet 34 is not opposite one of the openings 52 and the mobile part 50 is substantially in the axis XX ′ of flow of the fluid jet 22, and an open position, in which the outlet 34 is opposite one of the openings 52 and the movable part 50 allows the fluid jet 22 to flow without fractionation of the latter.
    The actuator is configured to move the movable part 50 between the open position and the closed position at a predetermined frequency, so as to fragment the fluid jet 22 and thus form the dispersion 12 according to the invention.
    The speed (or frequency) of movement of the mobile part 50 between the open position and the closed position, the dimensions of the mobile part 50 and / or of the opening 52, the spacing between the mobile part 50 and the opening 52 and / or the flow rates imposed on the first fluid 36 and on the second fluid 40 determine the size of the elements 14.
    According to this embodiment, the element 14 is single-phase and includes only the first fluid 36, and optionally a bark 16A as mentioned above.
    The volume of the elements 14 depends on the frequency of movement of the mobile part 50, the dimensions of the mobile part 50 and / or the opening 52, the spacing between the mobile part 50 and the opening 52 and / or flow rates imposed on the first fluid 36 and on the second fluid 40, and therefore on the fluid jet 22. In particular, the volume ratio of the elements 14 and of the continuous phase 18 depends on the ratio of the flow rates of the first fluid 36 and of the second fluid 40 to the outlet 34 of the nozzle 20.
    The adjustments to these various parameters depend on the general knowledge of the skilled person. In other words, a person skilled in the art will know how to make the necessary adjustments to form elements 14 of the desired size.
    The chamber 26 is intended to receive the dispersion 12 resulting from the fragmentation of the fluid jet 22 and to evacuate the dispersion 12 for distribution.
    The chamber 26 is located directly at the outlet 34 of the nozzle 20, so that the nozzle 20 opens directly into the receptacle 26 through the fragmentation device 24.
    According to an embodiment not shown, the device 10 further comprises at least one mixer into which the dispersion 12 is injected, capable of exerting a uniform and controlled shear on the elements 14. The mixer comprises at least one shear cell.
    The mixer is capable of improving the monodispersity of the elements 14, the elements 14 being subjected to shearing capable of fragmenting them into elements 14 of homogeneous and controlled diameters, as described in more detail in EP3144058. According to this embodiment, the dispersion 12 obtained comprises elements 14 endowed with an homogeneity of improved size.
    The shear cell is advantageously a Couette type cell, comprising at least two coaxial rotary cylinders. The cylinders comprise for example an external cylinder having an internal radius Ro and an internal cylinder having an external radius Ri, with Ro> Ri. The outer cylinder is for example fixed, and the inner cylinder is for example driven by a rotation movement at constant angular speed ω. Dispersion 12 is arranged between the outer cylinder and the inner cylinder, and sheared by the differential movement of the two cylinders.
    Alternatively, the shear cell comprises two parallel rotating discs, or two parallel oscillating plates.
    Other embodiments of the device 10
    According to an embodiment shown in FIG. 2, the device 10 further comprises at least one independent conduit 62 suitable for conveying at the level of the dispersion 12 at least one additional fluid 64 from an independent channel 66 for supplying additional fluid 64 comprising at least one solution for increasing the viscosity of the continuous phase 18. The second fluid 40 is therefore miscible with the additional fluid 64. Such a solution for increasing the viscosity is for example a solution containing a base, in particular a alkali hydroxide, such as sodium hydroxide, and is especially described in WO2015055748.
    According to another embodiment shown in FIG. 3, the movable part of the fragmentation device 24 comprises a rotary scraper 80 movable in rotation about a central axis Z-Z ’at a constant angular speed.
    The scraper 80 is for example a rotor with a hollow axis, substantially circular and has openings 82 oriented radially, opening onto an external contour 84 of the scraper 80. The openings 82 open into the recessed central part of the scraper 80. Advantageously, the openings 82 are evenly spaced along the outer contour 84.
    The external contour 84 extends in the vicinity of the outlet 34, and is orthogonal to the flow axis X-X ’, so that the external contour is substantially tangent to the plane of the opening 34.
    The fragmentation device 24 is thus movable by rotation about the central axis Z-Z ’between the open position in which one of the openings 82 is opposite the outlet 34 and the closed position, as described above.
    The actuator is for example an electric motor capable of driving the rotary scraper in rotation around the central axis Z-Z ’. The frequency of passage from the closed position to the open position then depends on the angular speed of rotation of the scraper 80 and on the angular difference between two successive openings 82.
    As a variant, the scraper 80 is driven by an oscillating movement rather than a rotary movement at constant angular speed.
    According to another embodiment illustrated in FIG. 4, the device 10 comprises a nozzle 20 comprising the first conduit 30 and the second conduit 32 as well as a third conduit 100. At least part of the third conduit 100 is preferably surrounded coaxially, by at least part of the first conduit 30. The third conduit 100 is suitable for conveying a third fluid 102, and supplied by a third channel 104 for supplying third fluid 102.
    According to a variant (not shown), the first conduit 30 and the third conduit 100, or even moreover the second conduit 32, open on the same plane, in particular at the outlet 34 of the nozzle 20.
    The fluid jet 22 then comprises the first fluid 36, the second fluid 40 surrounding the first fluid 36, preferably coaxially, and the third fluid 102 surrounded by the first fluid 36, preferably coaxially, the fluid jet 22 being formed by co-extrusion. Each of the elements 14 formed after fragmentation of the fluid jet 22 then comprises, at least temporarily, an outer core 110 formed by the first fluid 36, and at least one, preferably a single, inner core 112 formed by the third fluid 102, disposed in the outer heart 110.
    Indeed, according to a first variant, the third fluid 102 and the first fluid 36 are substantially miscible. This variant is advantageously in that it allows the encapsulation within the same phase of the raw materials which are not compatible with each other.
    Thus, by way of illustration of this first variant, in the case where the elements 14 comprise a coacervate bark 16A, the third fluid 102 comprises high contents of vegetable oils and the first fluid 36 comprises at least one lipophilic cationic polymer precursor of the coarcervate , in particular an amodimethicone, as described above, in an oil known to be a good solvent for the cationic polymer. Thus, any possible incompatibility between said cationic polymer and vegetable oil occurs after the formation of the coacervate bark.
    More generally, the third fluid 102 and the first fluid 36 each comprise active agents capable of reacting with one another; thus, these assets govern together after the formation of the elements 14.
    This makes it possible to form single-phase elements 14.
    According to a second variant, the third fluid 102 and the first fluid 36 are substantially immiscible. The dispersion 12 is thus multiple, in particular double, and in particular of the water-in-oil-in-water, oil-in-water-in-oil or oil-in-oil-in-water type. This makes it possible to form two-phase elements 14.
    According to a first example, the two-phase elements 14 form drops provided with a multicomponent heart, that is to say comprising an internal heart 112 formed by the third fluid 102 and an external heart 110 formed by the first fluid 36 surrounding completely the internal heart 112. Optionally, these drops comprise a shell, in particular of coacervate, as described above at the interface between the first fluid 36 and the continuous phase 18, or even moreover between the first fluid 36 and the third fluid 102 Such a drop is illustrated in Figure 5.
    According to another example (not shown), the two-phase elements 14 of the dispersion 12 comprises at least a first gelling agent in the first phase 16 and optionally at least a second gelling agent in the continuous phase 18. In other words, the diphasic elements 14 according to this second variant have improved kinetic stability and mechanical resistance despite the absence of bark and the gelation of the external heart 110 makes it possible to prevent creaming or sedimentation of the internal heart 112. Examples of gelling agents are described in the application filed under No. FR1752208.
    According to a third example, the elements 14 form drops based on a combination of the first and second examples above.
    According to a fourth example, the elements 14 form capsules comprising a heart 113 formed by the third fluid 102 and a bark 16C formed by the first fluid 36 disposed around the heart 113. Such a capsule is illustrated in FIG. 6.
    The bark can be produced from at least one gelling agent.
    Such a gelling agent may for example be chosen from a thermosensitive gelling agent which is solid at room temperature and atmospheric pressure, such as for example agar.
    Such a gelling agent may for example be chosen from a polysaccharide, in particular a polyelectrolyte reactive with multivalent ions, such as for example an alginate.
    The gelation of the polyelectrolyte requires the presence in the second fluid 40 of at least one reagent capable of reacting with the polyelectrolyte to make it pass from a liquid state to a gelled state. Such a reagent is typically a solution comprising multivalent ions such as ions of an alkaline earth metal chosen for example from calcium ions, barium ions, magnesium ions, and their mixtures. Examples of gelling agents, in particular heat-sensitive agents, of polysaccharides, in particular of polyelectrolytes reactive with multivalent ions, and of reagents capable of reacting with the polyelectrolyte to bring it from a liquid state to a gelled state are described in WO2010063937.
    Preferably, when the second fluid 40 comprises at least one reagent capable of reacting with the polyelectrolyte present in the first fluid 36 to make it pass from a liquid state to a gelled state, the first fluid 36 and / or the second fluid 40 comprises in addition at least gelling retardant, such as for example a tetrasodium pyrophosphate.
    According to another embodiment not shown, the device 10 further comprises at least one heating device suitable for heating at least the first fluid 36 and / or the second fluid 40 in the nozzle 20. The heating device is for example arranged in the vicinity of the first conduit 30 and / or the second conduit 32, and in particular surrounds the first conduit 30 and / or the second conduit 32, preferably in a coaxial manner. According to a first variant, the heating device comprises for example a heating resistor and an electric generator, and is capable of heating the first fluid 36 by the Joule effect. According to a second variant, the heating device comprises for example a heat exchanger.
    As a variant, the heating device is suitable for heating the third fluid 102, and is arranged in the vicinity of the third conduit 100, or alternatively is suitable for heating both the first fluid 36, the second fluid 40 and the third fluid 102 and located in the vicinity of the first conduit 30, the second conduit 32 and the third conduit 100.
    Production set 75
    Referring to Figure 3, there is described a production assembly 75 comprising a plurality of production devices 10 according to the first embodiment described above.
    The production devices 10 are arranged around at least one centripetal circle, with their respective flow axes X-X ’converging towards the center of the circle. In the example shown in Figure 3, the production devices 10 are arranged in a centripetal circle, the center of which is located on the central axis Z-Z ’.
    According to an embodiment not shown, the production devices 10 are arranged in at least two superimposed centripetal circles, the centers of which are aligned along the central axis Z-Z ’. Such an embodiment is advantageous in that it makes it possible to easily increase the production yields in dispersion 12 according to the invention, if necessary without multiplying the conduits 38, 42 and optionally 104 for supplying fluids, respectively. 36, 40 and 102.
    The outlets 34 of the devices 10 open into the same shared room 26, intended to receive the dispersion 12 produced by each of the devices 10.
    The production assembly 75 includes a fluid distribution system capable of supplying each production device 10 with the first fluid 36 with the second fluid 40, and optionally with the third fluid 102, via the first channels 38 and the second channels respectively. 42 and optionally third channels 104.
    Advantageously, the devices 10 share the same first channel 38 and the same second channel 42 and optionally the same third channel 104, the first channel 38 and the second channel 42 and optionally the third channel 104 being substantially circular and concentric with the centripetal circle.
    The fluid distribution system comprises for example a first pump fluidly connected to the first channel 38 and to a reservoir of first fluid 36. The first pump is suitable for circulating the first fluid 36 in the first channel 38 and for supplying the devices 10 first fluid 36 with predetermined flow.
    The fluid distribution system also comprises a second pump fluidly connected to the second channel 42 and to a reservoir of second fluid 40. The second pump is suitable for circulating the second fluid 40 in the second channel 42 and for supplying the devices 10 with second fluid 40 at a predetermined flow rate, equal or not to the flow rate of the first fluid 38.
    Optionally, the fluid distribution system also includes a third pump fluidly connected to the third channel 104 and to a reservoir of third fluid 102. The third pump is adapted to circulate the third fluid 102 in the third channel 104 and to supply the devices 10 in third fluid 102 at a predetermined flow rate, equal or not to the flow rate of the first fluid 36 and / or of the second fluid 40.
    The devices 10 advantageously share the same fragmentation device, which comprises a rotary scraper 80 as described above. The rotary scraper 80 is arranged to travel an internal contour 83 of the centripetal circle and thus be substantially tangent to the opening plane of each of the outlets 34 of the devices 10. The internal contour 83 of the centripetal circle and the external contour 84 of the scraper 80 are advantageously separated by a distance less than or equal to 1 mm, preferably less than or equal to 0.5 mm, and better still less than or equal to 0.2 mm.
    The openings 82 of the rotary scraper 80 are advantageously regularly angularly spaced, the rotary scraper is therefore suitable for fragmenting the fluid jets 22 formed by each of the nozzles 20 at the same predetermined frequency and thus forming the elements 14 identically at the outlet 34 of each of the nozzles 20.
    According to a variant (not shown), the production devices 10 of the assembly 75 are arranged around at least one centrifugal circle, with their respective flow axes X-X ′ diverging from the center of the circle.
    The outlets 34 of the devices 10 are oriented towards the outside of the centrifugal circle and open into the same shared, substantially annular chamber 26, arranged around the production devices 10.
    The fluid distribution system is as described above, the first channel 38, the second channel 42 and optionally the third channel 104 of fluid distribution being disposed internally relative to the production devices 10, for example in the vicinity of the central axis Z-Z '.
    The rotary scraper 80 is shared between the devices 10 and arranged to traverse an external contour of the centrifugal circle. An internal contour of the scraper 80 is thus substantially tangent to the outputs 34 of the devices 10, as described above.
    Production process
    A method for producing the dispersion 12 using the device 10 shown in FIG. 1 will now be described. The production process comprises a preliminary step of supplying the production device 10, as well as a first fluid 36 and a second fluid 40 substantially immiscible with the first fluid 36.
    Advantageously, the first fluid 36 is supplied via a first channel 38 for supplying the first fluid 36 fluidly connected to a first conduit 30 and the second fluid 40 is supplied via a second channel 42 d supply of second fluid 40 fluidly connected to a second conduit 32 of a nozzle 20 of the device 10.
    The method comprises at least one flow step, in the direction of an outlet 34 of the nozzle 20 in a flow direction XX ′, of the first fluid 36 in a first conduit 30 and of the second fluid 40 in a second conduit 32, said second conduit 32 surrounding, preferably coaxially, at least part of the first conduit 30.
    The method then comprises a step of forming a fluid jet 22 at the outlet 34 of the nozzle 20, the fluid jet 22 being formed by co-extrusion and comprising the first fluid 36 and the second fluid 40 surrounding the first fluid 36, preferably coaxially.
    Advantageously, the fluid jet 22 flows in the direction of flow X-X ’, and transversely to an opening plane of the outlet 34.
    The method comprises a step of moving a movable part 50 of a fragmentation device 24 of the production device 10, to fragment the fluid jet 22 and obtain a dispersion 12 according to the invention.
    Advantageously, the mobile part 50 is moved in a direction substantially orthogonal to the flow direction X-X ’, and substantially tangentially to the opening plane of the outlet 34.
    Advantageously, the movable part 50 is moved by an actuator so as to form the elements 14 at a predetermined fixed frequency. The elements 14 are then substantially identical to each other, so that the dispersion 12 obtained is monodisperse.
    Advantageously, the movable part 50 is a rotary scraper 80, the displacement of the movable part 50 is then a rotation about a central axis Z-Z ’at a constant angular speed. As a variant, the mobile part 50 is a scraper driven by an oscillating movement rather than a rotary movement at constant angular speed.
    An external contour 84 of the rotary scraper then extends in the vicinity of the outlet 34, in a manner substantially tangent to the opening plane of the outlet 34.
    The method finally comprises a step of recovering the dispersion 12 comprising the elements 14 dispersed in the continuous phase 18.
    In another embodiment, the method comprises the step of flowing the first fluid 36 and second fluid 40 as described above, as well as a third fluid 102 in a third conduit 100 surrounded at least in part, by preferably coaxially, by at least part of the first conduit 30.
    According to a first variant, the third fluid 102 is substantially miscible with the first fluid 36.
    According to a second variant, the third fluid 102 is substantially immiscible with the first fluid 36.
    The fluid jet 22 thus formed by co-extrusion comprises the first fluid 36, the second fluid 40 and the third fluid 102, in which the second fluid 40 surrounds the first fluid 36, preferably coaxially, and the first fluid 36 surrounds the third fluid 102, preferably coaxially.
    In the dispersion 12 thus obtained and according to the miscible or immiscible nature of the first fluid 36 and third fluid 102 therebetween, the elements 14 are single-phase or two-phase.
    In another embodiment, the method further comprises a size refining step, during which a controlled and homogeneous shear is applied to the elements 14 in a mixer, the mixer being in particular as described above.
    In another embodiment, the method further comprises a step of filtering the dispersion 12 to collect only the elements 14.
    Compounds and additional active ingredients
    A dispersion 12 according to the invention, in particular the dispersed phase 16 and / or the continuous phase 18 and / or the third fluid 102, may (may) also comprise at least one additional compound different from the precursor polymers of the coacervate, gelling agents, the above-mentioned polysaccharides.
    A dispersion 12 according to the invention, in particular the dispersed phase 16 and / or the continuous phase 18 and / or the third fluid 102, may (may) also comprise powders, flakes, coloring agents, in particular chosen from coloring agents, water-soluble or not, liposoluble or not, organic or inorganic, pigments, materials with optical effect, liquid crystals, and their mixtures, particulate agents insoluble in the fatty phase, silicone elastomers emulsifiers and / or not emulsifiers, preservatives, humectants, stabilizers, chelators, emollients, modifying agents chosen from agents of pH, osmotic force and / or modifiers of refractive index, etc. or any usual cosmetic additive, and their mixtures.
    A dispersion 12 according to the invention, in particular the dispersed phase 16 and / or the continuous phase 18 and / or the third fluid 102, can also (at least) include at least one active agent, in particular biological or cosmetic, preferably chosen among the hydrating agents, the healing agents, the depigmenting agents, the UV filters, the desquamating agents, the antioxidant agents, the active agents stimulating the synthesis of dermal and / or epidermal macromoleculars, the dermodecontracting agents, the antiperspirant agents, the agents soothing, anti-aging agents, perfuming agents and their mixtures. Such assets are described in particular in FR 1,558,849.
    Of course, the person skilled in the art will take care to choose any additional compound (s) mentioned above and / or their respective amounts so that the device and / or the advantageous properties of a dispersion according to the invention are not not or substantially not altered by the proposed addition. In particular, the nature and / or the amount of the additional compound (s) depends on the aqueous or oily (or fatty) nature of the phase in question of the dispersion according to the invention. These adjustments fall within the competence of a person skilled in the art.
    uses
    A dispersion according to the invention can be a topical composition, and therefore not an oral composition, or a food composition.
    Preferably, a dispersion according to the invention can be used directly, at the end of the aforementioned preparation processes, as a composition, in particular a cosmetic.
    The dispersions according to the invention can comprise, in addition to the abovementioned ingredients, at least one physiologically acceptable medium.
    In the context of the invention, and unless otherwise stated, the term “physiologically acceptable medium” means a medium suitable for cosmetic applications, and in particular suitable for applying a composition of the invention to a keratin material, in particular the skin and / or the hair, and more particularly the skin.
    The physiologically acceptable medium is generally adapted to the nature of the support on which the composition is to be applied, as well as to the appearance under which the composition is to be packaged.
    According to one embodiment, the physiologically acceptable medium is represented directly by the continuous phase as described above.
    The cosmetic compositions of the invention can be for example a cream, an emulsion, a lotion, a serum, a gel and an oil for the skin (hands, face, feet, etc.), a foundation (liquid, paste ) a preparation for baths and showers (salts, foams, oils, gels, etc.), a hair care product (hair dyes and bleaches), a cleaning product (lotions, powders, shampoos), a maintenance product for hair (lotions, creams, oils), a styling product (lotions, hairsprays, brilliants), a shaving product (soaps, mousses, lotions, etc.), a product intended to be applied to the lips, a product sunscreen, a sunless tanning product, a product for whitening the skin, an anti-wrinkle product. In particular, the cosmetic compositions of the invention can be an anti-aging serum, a youth serum, a hydrating serum or a scented water.
    The present invention also relates to a non-therapeutic method of cosmetic treatment of a keratinous material, in particular the skin and / or the hair, and more particularly the skin, comprising a step of applying to said keratinous material at least one composition or at least one layer of a cosmetic composition mentioned above.
    Throughout the description, the expression "comprising a >> should be understood as being synonymous with" comprising at least one >>, unless otherwise specified. The expressions "between ... and ... >>," between ... and ... >> and "ranging from ...
    to ... >> must be understood bounds included, unless otherwise specified.
    权利要求:
    Claims (17)
    [1" id="c-fr-0001]
    1. - Device (10) for producing a dispersion (12) comprising elements (14) comprising at least a first phase (16), dispersed in a continuous phase (18) substantially immiscible with the first phase (16), the device (10) comprising:
    - at least one production nozzle (20) comprising at least a first conduit (30) intended to convey a first fluid (36) capable of constituting the first phase (16), a second conduit (32) surrounding, preferably so coaxial, at least part of the first conduit (30), the second conduit (32) being able to convey a second fluid (40) capable of constituting the continuous phase (18), and an outlet (34), the nozzle (20 ) being adapted to form at the outlet (34) a fluid jet (22) comprising at least the first fluid (36) and the second fluid (40) surrounding the first fluid (36), preferably coaxially, and
    - at least one mechanical fragmentation device (24) of the fluid jet (22), disposed in the vicinity of the outlet (34) of the nozzle (20), the fragmentation device (24) comprising a movable part (50) relative to the nozzle (20), intended to mechanically fragment the fluid jet (22) into a plurality of elements (14) comprising the first fluid (36) dispersed in the continuous phase (18).
    [2" id="c-fr-0002]
    2. - Device (10) according to claim 1, wherein the production nozzle (20) comprises a third conduit (100) at least part of which is surrounded, preferably coaxially, by at least part of the first conduit (30), the third conduit (100) being adapted to convey a third fluid (102) substantially immiscible with the first fluid (36), the fluid jet (22) comprising the third fluid (102), the first fluid (36) surrounding the third fluid (102), preferably coaxially, and the second fluid (40) surrounding the first fluid (36), preferably coaxially, each element (14) dispersed in the continuous phase (18) comprising a outer core (110) formed by the first fluid (36), and at least one, preferably a single, inner core (112) formed by the third fluid (102) disposed in the outer core (110).
    [3" id="c-fr-0003]
    3. - Device (10) according to claim 1 or 2, wherein each element (14) comprises a bark (16A), preferably formed of a layer of coacervate, at the interface between the first phase (16) and the continuous phase (18), and optionally also at the interface between the first phase (16) and the third fluid (102).
    [4" id="c-fr-0004]
    4. - Device (10) according to claim 2, wherein the first phase (16) of the elements (14) forms a shell (16C) formed of a layer comprising at least one gelling agent, in particular chosen from a gelling agent thermosensitive solid at room temperature and atmospheric pressure, a polysaccharide, in particular a polyelectrolyte reactive with multivalent ions, between the third fluid (102) and the continuous phase (18).
    [5" id="c-fr-0005]
    5. - Device (10) according to any one of claims 1 to 4, in which the device (10) comprises at least one independent conduit (62) intended to convey to the dispersion (12) an additional fluid (64) comprising at least one solution for increasing the viscosity of the continuous phase (18).
    [6" id="c-fr-0006]
    6. - Device (10) according to any one of claims 1 to 5, wherein the device (10) comprises at least one heating device capable of heating at least the first fluid (36), and optionally the second fluid ( 40) and / or the third fluid (102), at least in the production nozzle (20).
    [7" id="c-fr-0007]
    7. - Device (10) according to any one of claims 1 to 6, wherein the movable part (50) of the fragmentation device (24) comprises a scraper (80) rotary or oscillating, provided with openings (82) successive.
    [8" id="c-fr-0008]
    8. - Device (10) according to any one of claims 1 to 7, wherein the elements (14) have a substantially spherical shape.
    [9" id="c-fr-0009]
    9. - Device (10) according to any one of claims 1 to 8, in which at least 60%, or even at least 70%, preferably at least 80%, and better still at least 90% of the elements (14) have an average diameter greater than or equal to 10 μm, preferably greater than or equal to 50 μm, in particular greater than or equal to 100 μm, or even greater than or equal to 200 μm, better still greater than or equal to 300 μm, and in particular greater than or equal at 400 pm.
    [10" id="c-fr-0010]
    10. - Device (10) according to any one of claims 1 to 9, the device (10) further comprising at least one mixer capable of exerting on the elements (14) a homogeneous controlled shear, said mixer comprising at least one cell formed by at least:
    - two coaxial rotary cylinders;
    - two parallel rotating discs; or
    - two parallel oscillating plates.
    [11" id="c-fr-0011]
    11, - assembly (75) for producing a dispersion (12) comprising a plurality of production devices (10) according to any one of claims 1 to 10 and a fluid distribution system capable of supplying each device (10 ) at least first fluid (36) and second fluid (40) and, optionally, third fluid (102), preferably the outlets (34) of the nozzles (20) opening into the same chamber (26).
    [12" id="c-fr-0012]
    12, - assembly (75) according to claim 11, wherein the devices (10) are arranged in at least one centripetal circle, the outlets (34) of the nozzles (20) being oriented towards a center of the circle.
    [13" id="c-fr-0013]
    13, - assembly (75) according to any one of claims 11 and 12, wherein the fragmentation device (24) is common to all the devices (10).
    [14" id="c-fr-0014]
    14, - assembly (75) according to claims 12 and 13, wherein the movable part (50) of the common fragmentation device (24) comprises a rotary or oscillating scraper (80) arranged to traverse an internal contour (83) of the circle centripetal.
    [15" id="c-fr-0015]
    15, - Method for manufacturing a dispersion (12) comprising elements (14) comprising at least a first phase (16) dispersed in a continuous phase (18), the method comprising at least the following steps:
    - supply of a production device (10) according to any one of claims 1 to 10 and of at least a first fluid (36) and a second fluid (40) substantially immiscible with the first fluid (36);
    - flows of the first fluid (36) in the first conduit (30), the first fluid (36) forming the first phase (16) and of the second fluid (40) in the second conduit (32) surrounding, preferably coaxially , the first conduit (30);
    - formation of a fluid jet (22) at the outlet (34) of the nozzle (20), the fluid jet (22), formed by co-extrusion, comprising at least the first fluid (36) and the second fluid (40 ) surrounding the first fluid (36), preferably coaxially;
    - displacement of the mobile part (50) of the fragmentation device (24) to fragment the fluid jet (22) and obtain elements (14) comprising at least the first fluid (36) dispersed in the second fluid (40); and
    - recovery of the dispersion (12).
    [16" id="c-fr-0016]
    16. - The method of claim 15, further comprising a step of flowing a third fluid (102) in a third conduit (100), at least part of the third conduit (100) being surrounded, preferably so coaxial, through at least a portion of the first conduit (30), the fluid jet (22) also comprising the third fluid (102), the first fluid (36) surrounding the third fluid (102), preferably coaxially.
    [17" id="c-fr-0017]
    17, - Method according to any one of claims 15 to 16, comprising a step of refining in size, during which a controlled and homogeneous shearing is applied to the elements (14) in a mixer, the mixer being in particular of the type Duvet, comprising two coaxial cylinders, an external cylinder of internal radius R o and an internal cylinder of external radius R ,, the external cylinder being fixed and the internal cylinder being in rotation with an angular speed ω.
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    同族专利:
    公开号 | 公开日
    WO2019145424A1|2019-08-01|
    CN112203754A|2021-01-08|
    FR3077011B1|2020-02-14|
    US20210039059A1|2021-02-11|
    EP3743201A1|2020-12-02|
    KR20200108473A|2020-09-18|
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    EP3144058A1|2015-09-16|2017-03-22|Calyxia|Method for preparing microcapsules by double emulsion|CN111569759A|2020-05-21|2020-08-25|陈晨|High efficiency chemical fertilizer processingequipment|
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    法律状态:
    2018-12-14| PLFP| Fee payment|Year of fee payment: 2 |
    2019-07-26| PLSC| Publication of the preliminary search report|Effective date: 20190726 |
    2019-12-12| PLFP| Fee payment|Year of fee payment: 3 |
    2020-12-30| PLFP| Fee payment|Year of fee payment: 4 |
    2021-12-10| PLFP| Fee payment|Year of fee payment: 5 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1850550|2018-01-24|
    FR1850550A|FR3077011B1|2018-01-24|2018-01-24|DEVICE FOR PRODUCING A DISPERSION, ASSEMBLY AND ASSOCIATED METHOD|FR1850550A| FR3077011B1|2018-01-24|2018-01-24|DEVICE FOR PRODUCING A DISPERSION, ASSEMBLY AND ASSOCIATED METHOD|
    KR1020207023997A| KR20200108473A|2018-01-24|2019-01-24|Apparatus, associated assemblies and associated methods for making dispersions|
    PCT/EP2019/051756| WO2019145424A1|2018-01-24|2019-01-24|Device for producing a dispersion, associated assembly and associated method|
    EP19700971.5A| EP3743201A1|2018-01-24|2019-01-24|Device for producing a dispersion, associated assembly and associated method|
    CN201980015350.6A| CN112203754A|2018-01-24|2019-01-24|Device for producing a dispersion, associated assembly and associated method|
    US16/964,025| US20210039059A1|2018-01-24|2019-01-24|Device for producing a dispersion, associated assembly and associated method|
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