EP1551540A1 - Method and device for making a dispersion or an emulsion - Google Patents

Method and device for making a dispersion or an emulsion

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Publication number
EP1551540A1
EP1551540A1 EP03778394A EP03778394A EP1551540A1 EP 1551540 A1 EP1551540 A1 EP 1551540A1 EP 03778394 A EP03778394 A EP 03778394A EP 03778394 A EP03778394 A EP 03778394A EP 1551540 A1 EP1551540 A1 EP 1551540A1
Authority
EP
European Patent Office
Prior art keywords
porous
coφs
emulsion
fluid
porous body
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP03778394A
Other languages
German (de)
French (fr)
Other versions
EP1551540B1 (en
Inventor
Christopher Arnaud
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ARNAUD, CHRISTOPHE
Original Assignee
Individual
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Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of EP1551540A1 publication Critical patent/EP1551540A1/en
Application granted granted Critical
Publication of EP1551540B1 publication Critical patent/EP1551540B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
    • B01F25/31421—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction the conduit being porous
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B01F23/411—Emulsifying using electrical or magnetic fields, heat or vibrations
    • B01F23/4111—Emulsifying using electrical or magnetic fields, heat or vibrations using vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/49—Mixing systems, i.e. flow charts or diagrams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • B01F31/84—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations for material continuously moving through a tube, e.g. by deforming the tube
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S516/00—Colloid systems and wetting agents; subcombinations thereof; processes of
    • Y10S516/924—Significant dispersive or manipulative operation or step in making or stabilizing colloid system
    • Y10S516/928—Mixing combined with non-mixing operation or step, successively or simultaneously, e.g. heating, cooling, ph change, ageing, milling

Definitions

  • the present invention relates to a device and a method for manufacturing a dispersion or an emulsion of at least two fluids deemed immiscible.
  • the manufacture of a dispersion or emulsion is the mixture of two immiscible fluids in which one of these fluids (called “dispersed phase”) is dispersed in the form of droplets in the other fluid (called “dispersing phase”). ").
  • the size of the droplets depends on many properties, and in general, the smaller and more homogeneous the size, the more interesting the dispersion: the smaller the droplets, the more stable the dispersion; in the classical case where the dispersed phase is the vector of an active ingredient, the smaller the drops, the better the diffusion of the active ingredient.
  • a ring In the rotor-stator systems, a ring is rotated relative to another and the fluid to be treated is passed between the surfaces facing each other of these two rings. Thus the difference in speed between the crowns creates a shear that is optimized by decreasing the distance between the two crowns.
  • rotor-stator devices There are many geometries of rotor-stator devices, some systems include several rows of crowns. These systems widespread in the industry are particularly suitable for dispersions of high viscosity. Pressure vessels, homogenizers, devices known as Microfluidizer (registered trademark) and other jet devices are the subject of the most recent developments.
  • the principle is the pressurization (up to 200 MPa) of a fluid, which is generally a pre-dispersion followed by a sudden expansion in a suitable head, thus bringing the fluid a significant mechanical energy.
  • the homogenizers have a head formed of an opening, a valve and impact plates.
  • the principle of the Microfluidizer (registered trademark) is to separate the main flow and then to create a secondary flow collision.
  • Devices based on these principles are confronted with equipment resistance limits (high wear, risk of rupture of a material under heavy stress).
  • the very principle of relaxation causes a heating of the fluid which can be detrimental to the final product.
  • Ultrasound is also a means of exerting a mechanical action at the interface of the two phases.
  • ultrasound generators the first called transducers convert an oscillating electrical signal into ultrasonic vibration; the second called whistles transform the energy of a fluid jet into ultrasonic vibrations, on the principle of a vibrating blade or a resonant cavity.
  • Another emulsion manufacturing system is the membrane emulsification: the dispersed phase which forms drops on the surface of this body is pushed through a porous body, the dispersant phase flow on the surface of the porous body allows the training of the drops.
  • the energy transmitted to the interface is limited by the losses due to friction in the dispersant phase; as a result the entrained drops are of larger size (approximately 4-5 times the pore size) and a phenomenon of coalescence on the surface of the porous body occurs increasing the size of the drops and the inhomogeneity of the droplet populations.
  • the phenomenon of coalescence occurs when at least two drops formed on neighboring pores combine to form one.
  • a solution to this last disturbing phenomenon is envisaged in the JP2-214537 patent. It consists of the addition of an ultrasonic irradiation of the porous body.
  • the wave generated by a standard washing system is transmitted in a fluid way.
  • More volumes in which mechanical energy is supplied are greater than 10 "10 m 3 for actions on useful volumes (particle size in dispersion, cells ...) typically of the order of 10" m.
  • the devices used can not ensure the homogeneity of the mechanical action, its effects and therefore the product obtained.
  • the purpose of the invention is to propose a process for manufacturing a dispersion or an emulsion of at least two fluids that are considered immiscible, which avoids the aforementioned drawbacks and allows the manufacture of a homogeneous emulsion or dispersion. with fine drops.
  • the object of the invention is also to propose a device implementing this method, by exerting a mechanical action directly at the interface of the two phases, which makes it possible to obtain finer and more homogeneous dispersions with better energy efficiency.
  • the subject of the invention is a process for producing a dispersion or an emulsion from at least two known immiscible fluids constituting a dispersed phase and a dispersant phase, the dispersed phase being pushed through a porous body in the dispersing phase, characterized in that said porous body is vibrated by an excitation of mechanical, electrical or magnetic nature.
  • the dispersant phase flows to the exit surface of the porous body.
  • the emulsion is re-circulated in the porous body which is charged in dispersed phase during the process.
  • the frequencies and / or the power of the vibrations are controlled.
  • an emulsifier is added in at least one of the two phases.
  • the dispersed phase is pushed through the porous body under conditions of controlled temperature, pressure, flow, composition, and agitation.
  • the dispersant phase circulates on the surface of the porous body under conditions of controlled temperature, pressure, flow, composition and agitation.
  • the process consists in using said dispersion or emulsion to produce cosmetic, dermopharmaceutical or pharmaceutical products.
  • the invention also relates to a device for the manufacture of a dispersion or an emulsion from at least one fluid comprising at least: a porous body having a porous portion through which is able to be pushed said fluid, said porous body having a so-called internal cavity, a casing sealingly surrounding at least said porous portion so as to define a so-called external cavity in which said porous part opens, said fluid being able to be brought into said external cavity, characterized in that it comprises a system for vibrating the porous body
  • "directly" is used in the sense or, contrary to the prior art, the vibrations are not essentially transmitted via one of the fluids.
  • the device can be applied to the manufacture of an emulsion or a dispersion from two fluids deemed immiscible or homogenization of an emulsion or dispersion from the same fluid.
  • the device comprises a supply system for said fluid capable of supplying said fluid in the external cavity under conditions of controlled temperature, pressure, flow, composition and agitation.
  • the device comprises a supply system for another fluid capable of supplying this other fluid in said internal cavity under conditions of controlled temperature, pressure, flow, composition and agitation.
  • the device comprises a withdrawal system for evacuation, and storage or transmission of the emulsion or dispersion to another system or the recirculation of the emulsion or dispersion.
  • the system for vibrating the porous body consists of a winding connected to a source of alternating current surrounding the envelope permeable to the magnetic waves generated by the winding, the porous body being made of magnetostrictive material.
  • the system for vibrating the porous body consists of a conductive rod disposed coaxially with the porous body, a conductive envelope, said conductive rod and said envelope being connected to an alternating current source, the porous body being made of a piezoelectric material.
  • the conductive rod and / or the surface of the porous body are covered with an insulator.
  • the system for vibrating the porous body consists of two transducers attached to the ends of the porous body and connected to an AC source, said transducers being made of a piezoelectric material.
  • each transducer comprises a support means attached to the casing having a recess in which is positioned an end of the porous body, said support means comprising at least one pair of radial holes, each pair containing a piezoelectric element in a hole and elastic biasing means in the other hole of the same pair for holding the piezoelectric element in abutment against the porous body, the holes of the same pair being diametrically opposed.
  • the support means comprises two pairs of holes, the two pairs of holes being arranged in perpendicular directions, and the two piezoelectric elements are powered by signals shifted by a quarter of a period relative to one another. and other, and in combination with the prestressing springs, cause a displacement of the porous body in a generally circular path.
  • FIG. 1 represents a longitudinal section of a module containing the porous body and a magnetic excitation means, and a section along the axis A-A of this module
  • Figure 2 is a longitudinal section of a module containing the porous body and an electrical excitation means, and a section along the axis A-A of this module
  • - Figure 3 is a longitudinal section of a module containing the porous body and a mechanical excitation means, and a section along the axis A-A of this module
  • Figure 4 is a schematic representation of an implementation of the invention
  • - Figure 5 is a schematic representation of an implementation of the invention with re-circulation of the emulsion or dispersion
  • Figure 6 is a detailed schematic representation of the device shown in Figure 5;
  • FIG. 1 represents a longitudinal section of a module containing the porous body and a magnetic excitation means, and a section along the axis A-A of this module
  • Figure 2 is a longitudinal section of a module containing the porous body
  • FIG. 7 is a longitudinal section of a module containing the porous body and a mechanical excitation means according to a second embodiment
  • Figure 8 is a perspective view of a coupling sleeve
  • - Figure 9 is a section along the axis IX of Figure 7 of a module containing the porous body and a mechanical excitation means
  • Fig. 10 is a diagram showing the results of the application example. - DESCRIPTION -
  • the device is in the form of active module 2, 102 and 202.
  • this module 2 is composed of a porous body 24, a coil 27 and a casing 23.
  • the porous body 24 is in the form of a hollow cylinder whose central porous portion 42 is included in FIGS. the envelope 23 of form cylindrical coaxial with porous co ⁇ s 24. The space between the porous co ⁇ s 24 and the envelope 23 defines an external cavity 21.
  • the casing 23 is connected to the ends 43 of the porous co ⁇ s 24 by a sealing system 25 and 25 '.
  • An internal cavity 22 is also defined inside the porous body 24.
  • the coil 27 connected to a source of alternating current 4 of adjustable power and frequency produces an oscillating magnetic field.
  • the porous co ⁇ s 24 is made in a magnetostrictive material and the envelope 23 in a material permeable to the magnetic waves produced by the coil 27.
  • the dispersed phase 40 is fed through the orifice 26 into the external cavity 21, then it is pushed through the porous portion 42 to the internal cavity 22, at the so-called outlet surface where it will be placed in contact. with the dispersing phase 44 flowing from the left end 43 of the porous co ⁇ s to that of the right. Contacting the dispersed phase 40 in the form of droplets after passing through the porous part 42 and the dispersing phase 44 is at the base of the emulsion or dispersion 41.
  • the envelope 23 serves to comprise the dispersed phase 40 which will be pushed through the porous co ⁇ s 24 and allow the vibrations of the porous co ⁇ s 24 without degradation thereof.
  • the sealing system 25 and 25 ' may advantageously be composed of two flexible joints ensuring both the sealing and the mobility of the porous body with respect to the envelope 23.
  • the embodiment shown in FIG. of vibrating 51 by magnetic excitation that is to say that the system 51 is composed of the alternating current source 4 connected to the coil 27 whose geometry makes it possible to exert on the porous co ⁇ s 24 an alternating magnetic field.
  • the porous body 24 thus subjected to an oscillating magnetic field vibrates and exerts on the interface of the two phases 40 and 44, the desired mechanical action.
  • the embodiment shown in FIG. 2 illustrates a vibrating system 151 by electrical excitation.
  • the identical elements will bear the same references and will not be described again.
  • the active module 102 differs from that shown in FIG. 1 only by the vibrating system.
  • the vibrating system 151 then comprises an alternating current source 4 connected to conductive surfaces between which the porous co ⁇ s 24 is placed.
  • the conductive surfaces consist of the conductive layer 46 of the envelope 23 and a conducting rod 28 placed coaxially with the cylinder formed by the porous co ⁇ s 24.
  • Each of the conductive surfaces 46 and 28 is connected to a terminal of an alternating current source 4 of adjustable power and frequency creating an oscillating electric field.
  • the conducting rod 28 is made of a conductive material advantageously covered with an insulating layer 45, just as the envelope 23 comprises at least one conductive layer 46 advantageously covered with an insulator 47 (represented by the thick black line defining the outline of the external cavity 21).
  • FIG. 3 illustrates a mechanical excitation vibration system 251.
  • the active module 202 differs from that shown in Figures 1 and 2 only by the vibrating system.
  • the vibrating system 251 then comprises an alternating current source 4 and 4 'connected to one or more coupled mechanical vibrators (mechanical connection) with the porous co ⁇ s 24, which may advantageously be fixed collar-shaped transducers 29 and 29' at the ends 43 of the porous co ⁇ s 24. These transducers 29 and 29 'directly transmit the vibrations to the porous co ⁇ s 24.
  • the system formed by the transducers 29 and 29 'and the porous co ⁇ s 24 forms an oscillator thus exerting the desired mechanical action at the dispersed phase 40 and dispersant 44 interface.
  • the transducers 290 and 290 ' are placed at each end 43 of the porous co ⁇ s 24 fixedly against the casing 23 and the sealing system 25 and 25'.
  • the transducers 290 and 290 ' are formed of a support means 291 and 291' for example in the form of an octagonal collar having a recess 52 coaxial with the X axis and according to Figure 9, two radial tapped holes 293a and 293b.
  • the end 43 of the porous co ⁇ s 24 is nested in a connecting sleeve 292 or 292 'itself placed in the coaxial recess 52.
  • This coupling sleeve 292 according to FIG.
  • each hole 293a and 293b is placed a piezoelectric element 294 and a prestressing spring 295 on either side of the connecting sleeve 292.
  • Four adjustment screws 296a, 296b, 296c and 296d close off the ends of each hole 293a and 293b.
  • the prestressing springs 295 are prestressed in compression by means of the four screws 296a, 296b, 296c and 296d mentioned above.
  • the piezoelectric elements 294 are powered by two periodic electric signals in quadrature with respect to each other (ie: shift of a quarter period) and undergo an elongation proportional to the supply voltage.
  • the input signal is rarely pure, it is up to say that it further comprises the main signal at a given frequency, other signals secondary to other frequencies, the movements then described by the transverse sections of the porous co ⁇ s 24 are composed of a sum of circular trajectories (corresponding each at a frequency of the input signal), guaranteeing on a section a global circular trajectory.
  • the two input signals on the two piezoelectric elements are identical to the nearest quarter of a period, to ensure that each point of the porous body 24 at a given cross-section undergoes the same vibrations and thus guarantee homogeneity of mechanical action.
  • the transducers 290 and 290 ' are powered by separate frequency signals each corresponding to a specific mode of the system. This allows an optimization and a good control of the generation of the vibrations, while avoiding the nodes of vibration where the mechanical action would be absent.
  • the device comprises an active module 2 connected by the pipe 5 to the supply system 1 in dispersed phase 40, via the pipe 7 to the supply system 8 in the dispersing phase 44 and through the pipe 6 to the withdrawal system 3.
  • the active module 2 is also connected to an alternating current source 4.
  • the AC source 4 supplies the active module 2 with the energy necessary to generate the mechanical action necessary for the generation of fine droplets.
  • the withdrawal system 3 connected to the active module 2 via the pipe 6 allows the evacuation of the emulsion or dispersion 41 of the porous co ⁇ s 24.
  • a variant of this implementation, shown in FIG. 5, comprises the same elements as in the previous embodiment, except that a pipe 17 connects the withdrawal system 3 to the module 2.
  • the withdrawal system 3 then allows the return of the emulsion or dispersion 41, thus creating a recirculation.
  • the draw-off system 3 is composed of at least one tank 30 and a pump 33 located between this tank 30 and the pipe 17.
  • the tank 30 is provided with a stirring system 31 and a system for maintaining the temperature 50 composed of a thermostated bath 35 and an exchange coil 34.
  • the disperse phase feed system 40 comprises a feed 48 of pressurized gas composed of a reservoir 13 (pressurized bottle, or compressor coupled to an expansion vessel) and a pressure reducer 14.
  • the system 1 comprises also a disperse phase reservoir 40, pressurizable, provided with a stirring system 11, and mounted on a scale or balance 15.
  • the system 1 finally comprises a shutoff valve 12.
  • the pressure regulator 14 can set the pressure to which is pushed the dispersed phase 40 at the level of the feed system 1.
  • the active module used corresponds to that shown in FIG. 3 with an embodiment identical to that of FIG. 6.
  • the active module can advantageously be a single-channel tangential filtration module adapted to the application, using porous co ⁇ s made of hydrophilic ceramic. with a pore diameter of 0.1 ⁇ m and 0.8 ⁇ m.
  • a hollow cylindrical porous co ⁇ s of length between 20 and 30 mm and outer radius between 10 and 15 mm and inner radius between 7 and 12 mm will be used.
  • the exemplary embodiment relates to the manufacture of an emulsion 41 of the oil-in-water type, composed for example of 10% of soybean oil, 0.5% of Tween 20 (registered trademark) and 89.5 emulsifier. % of water. A mixture of 4.8% Tween 20 and 95.2% oil is made in the tank 10 with stirring. Then a quantity of water X is circulated from the tank 30. Once the valve 12 is closed, the expander 14 is set to a pressure between 0.1 and 5 bar.
  • the transducers 29 and 29 ' are independently powered with the AC source 4 (composed of two separate sources) with power signals between 0 W and 2 kW and two frequencies one of which is between 14 and 16 kHz and the second between 18 and 22 kHz. Then the valve 12 is opened and closed when the amount of oil + emulsifier mixture reaches 0,1173X. During the entire operation, the temperature is maintained around a set temperature of between 15 and 25 ° C.
  • FIG. 10 diagram presenting the percentage by volume of the droplet populations according to their size. (in logarithmic scale).
  • the population distribution is represented by a broken line for the vibration-free test and a continuous line for the vibration test. In each case, we can observe the presence of several droplet populations, identified by several peaks. The presence of these same populations of drops has been confirmed by images taken with an electron microscope (images not shown).
  • an emulsion 41 whose drop size is less than 300 nm is obtained (results not shown). It may be advantageous to apply this example in particular to the manufacture of cosmetic, dermo-pharmaceutical or pharmaceutical products.
  • the vibrations of the exit surface of the porous co ⁇ s 24 act in this invention, releasing a mechanical energy of rupture directly at the dispersed and dispersive phase interface 44, making it possible to avoid the formation of large drops and generating the formation of fines. drops of dispersed phase 40 in the dispersing phase 44 at the base of the emulsion 41.
  • the system thus makes it possible to transmit at the interface of the two phases 40 and 44 a large amount of energy; the transmission being done by a solid (the porous co ⁇ s 24) and not by the fluids. It seems that under these conditions the phenomena of coalescence are inhibited, and the mechanism of formation and tearing drops accelerated. This hypothesis must, however, in no way be considered as limiting the invention.
  • the choice of the vibrating mode imposes magnetostrictive, piezoelectric or electrostrictive properties at the porous co ⁇ s. Other properties, geometric, mechanical, physico-chemical, chemical are determined by the application.
  • the general shape of the porous co ⁇ s 24 must optimize the surface through which the dispersed phase 40 passes while facilitating the transmission or generation of vibrations.
  • the hollow cylinder (we then take the principle of tangential filtration membrane assembly), is the one that has been presented previously.
  • a solid cylinder placed in a pipe may also be mentioned, the dispersed phase flowing in accordance with the axis of the cylinder, or a plug fixed in a pipe, and whose outlet surface is flush with the inner surface of a stirred tank.
  • the porosity, the pore size and the thickness of the porous co ⁇ s 24 determine the effective volume, and the duration of the mechanical action.
  • the mechanical resistance and the elasticity play on the amplitude of the vibrations and thus the intensity of the mechanical action.
  • the hydrophilic / hydrophobic character can substantially modify the fluid paths through the co ⁇ s but also the porous co ⁇ s interface 24 // dispersed phase 40 // dispersant phase 44 (contact angle).
  • a co ⁇ s 24 having a good affinity with the dispersing phase 44 is thus advantageously chosen in order to favor the separation of the drops of disperse phase 40. It is also necessary that the chosen materials be compatible with the products used. By using a co ⁇ s not permeable to microwaves it is impossible to heat this co ⁇ s and add to the mechanical effect a thermal effect.
  • the porous co ⁇ s 24 is not necessarily homogeneous.
  • a part of the co ⁇ s 24 located at its ends 43 may be non-porous.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Colloid Chemistry (AREA)
  • Medicinal Preparation (AREA)
  • Accessories For Mixers (AREA)

Abstract

Production of a mixture or an emulsion of at least two immiscible liquids is characterized by the fact that the dispersed phase is passed through a porous body (24) into the dispersing phase, and the porous body is vibrated by mechanical, electrical or magnetic excitation. Preferred Features: The dispersing phase circulates to the surface of the porous body (24) and is recirculated into the dispersed phase during the process. The frequency and the power of the vibrations are controlled. An emulsifier is added into one of the two phases. The dispersed phase is passed through the porous body (24) under controlled conditions of temperature, pressure and flow rate, and mixing. Likewise, the dispersing phase is circulated to the surface of the porous body (24) under controlled conditions of temperature, pressure and flow rate, and mixing. A wave selected from the microwave range and used for heating the porous body (24) is superposed on the vibration-generating waves. An Independent claim is given for a device for implementation of the invented process.

Description

PROCÉDÉ ET DISPOSITIF DE FABRICATION D'UNE DISPERSION OU D'UNE EMULSIONMETHOD AND DEVICE FOR MANUFACTURING A DISPERSION OR EMULSION
- OBJET ET DOMAINE DE L'INVENTION - La présente invention concerne un dispositif et un procédé de fabrication d'une dispersion ou d'une emulsion d'au moins deux fluides réputés non miscibles. La fabrication d'une dispersion ou d'une emulsion est le mélange de deux fluides non miscibles dans lequel l'un de ces fluides (appelé « phase dispersée ») est dispersé sous forme de gouttelettes dans l'autre fluide (appelé « phase dispersante »). De la taille des gouttelettes dépendent de nombreuses propriétés, et de façon générale plus cette taille est faible et homogène plus la dispersion est intéressante : plus les gouttelettes sont petites plus la dispersion est stable ; dans le cas classique où la phase dispersée est le vecteur d'un principe actif, plus petites sont les gouttes, meilleure est la diffusion du principe actif.OBJECT AND FIELD OF THE INVENTION The present invention relates to a device and a method for manufacturing a dispersion or an emulsion of at least two fluids deemed immiscible. The manufacture of a dispersion or emulsion is the mixture of two immiscible fluids in which one of these fluids (called "dispersed phase") is dispersed in the form of droplets in the other fluid (called "dispersing phase"). "). The size of the droplets depends on many properties, and in general, the smaller and more homogeneous the size, the more interesting the dispersion: the smaller the droplets, the more stable the dispersion; in the classical case where the dispersed phase is the vector of an active ingredient, the smaller the drops, the better the diffusion of the active ingredient.
- ÉTAT DE LA TECHNIQUE - Pour obtenir une certaine finesse de gouttes, il est connu d'utiliser une action mécanique d'agitation, en particulier par l'utilisation d'agitateurs à mobile tournant, d'appareils rotor - stator, d'appareils à pression, d'homogénéisateurs et autres appareils à jet, d'appareils à ultrasons, d'appareils d'émulsification membranaire.STATE OF THE ART In order to obtain a certain fineness of drops, it is known to use a mechanical stirring action, in particular by the use of rotary stirrers, rotor-stator apparatus and apparatus. pressure generators, homogenizers and other jet apparatus, ultrasonic apparatus, membrane emulsification apparatus.
Les agitateurs à mobile tournant sont les plus anciens, on en connaît bien le fonctionnement et les effets mécaniques ; de nombreuses études sur l'influence de la géométrie des récipients et mobiles, ainsi que des vitesses d'agitations ont été réalisées. L'énergie mécanique dispensée est très inhomogène et les puissances volumiques limitées. De plus, l'effet mécanique n'est concentré qu'aux extrémités du mobile.Mobile stirrers are the oldest, we know the operation and mechanical effects; many studies on the influence of the geometry of containers and mobiles, as well as speeds of agitations have been realized. The mechanical energy dispensed is very inhomogeneous and the power limited. In addition, the mechanical effect is concentrated only at the ends of the mobile.
Dans les systèmes rotor-stator on met en rotation une couronne par rapport à une autre et on fait passer le fluide à traiter entre les surfaces se faisant face, de ces deux couronnes. Ainsi la différence de vitesse entre les couronnes crée un cisaillement que l'on optimise en diminuant la distance entre les deux couronnes. Il existe de nombreuses géométries des appareils rotor-stator, certains systèmes comprennent plusieurs rangées de couronnes. Ces systèmes répandus dans l'industrie sont notamment adaptés aux dispersions de forte viscosité. Les appareils à pression, les homogénéisateurs, les appareils connus sous le nom Microfluidizer (marque déposée) et autres appareils à jet font l'objet des évolutions les plus récentes. Le principe en est la mise sous pression (jusqu'à 200 MPa) d'un fluide, qui est généralement une pré-dispersion suivie d'une détente brutale dans une tête adaptée, apportant ainsi au fluide une énergie mécanique importante. Les homogénéisateurs possèdent une tête formée d'une ouverture, d'un clapet et de plaques d'impact. Le principe du Microfluidizer (marque déposée) est de séparer le flux principal et ensuite de créer une collision des flux secondaires. On citera également un système basé sur la mise sous pression de la phase dispersée, sa détente brutale en un jet cohérent et enfin sa mise en contact avec la phase dispersante. Les dispositifs basés sur ces principes sont confrontés aux limites de résistance des équipements (forte usure, risque de rupture d'un matériel sous fortes contraintes). De plus, le principe même de détente provoque un échauffement du fluide qui peut être préjudiciable pour le produit final.In the rotor-stator systems, a ring is rotated relative to another and the fluid to be treated is passed between the surfaces facing each other of these two rings. Thus the difference in speed between the crowns creates a shear that is optimized by decreasing the distance between the two crowns. There are many geometries of rotor-stator devices, some systems include several rows of crowns. These systems widespread in the industry are particularly suitable for dispersions of high viscosity. Pressure vessels, homogenizers, devices known as Microfluidizer (registered trademark) and other jet devices are the subject of the most recent developments. The principle is the pressurization (up to 200 MPa) of a fluid, which is generally a pre-dispersion followed by a sudden expansion in a suitable head, thus bringing the fluid a significant mechanical energy. The homogenizers have a head formed of an opening, a valve and impact plates. The principle of the Microfluidizer (registered trademark) is to separate the main flow and then to create a secondary flow collision. There is also a system based on the pressurization of the dispersed phase, its sudden expansion into a coherent stream and finally its contact with the dispersant phase. Devices based on these principles are confronted with equipment resistance limits (high wear, risk of rupture of a material under heavy stress). In addition, the very principle of relaxation causes a heating of the fluid which can be detrimental to the final product.
Les ultrasons constituent également un moyen d'exercer une action mécanique à l'interface des deux phases. Plusieurs types de générateurs d'ultrasons existent : les premiers appelés transducteurs transforment un signal électrique oscillant en vibration ultrasonore ; les seconds appelés sifflets transforment l'énergie d'un jet fluide en vibrations ultrasonores, sur le principe d'une lame vibrante ou d'une cavité résonnante.Ultrasound is also a means of exerting a mechanical action at the interface of the two phases. Several types of ultrasound generators exist: the first called transducers convert an oscillating electrical signal into ultrasonic vibration; the second called whistles transform the energy of a fluid jet into ultrasonic vibrations, on the principle of a vibrating blade or a resonant cavity.
Plusieurs effets sont associés aux ultrasons : - L'agitation (micro-courants) provoquée par les oscillations mécaniques ;Several effects are associated with ultrasound: - agitation (micro-currents) caused by mechanical oscillations;
Les variations de pression dans le milieu soumis aux ultrasons ;Pressure variations in the medium subjected to ultrasound;
La cavitation, phénomène de création, oscillation et implosion de bulles, qui libère une énergie très importante ;Cavitation, phenomenon of creation, oscillation and implosion of bubbles, which releases a very important energy;
L'avantage de tels systèmes est d'arriver à des énergies volumiques très élevées. Cependant l'énergie est apportée de façon très inhomogène et le phénomène de cavitation n'est pas encore complètement décrit par la théorie, ce qui oblige dans le développement de dispositifs et de procédés à adopter des approches essentiellement empiriques. Un autre système de fabrication d'émulsion est l'émulsification membranaire: on pousse au travers d'un corps poreux la phase dispersée qui forme des gouttes à la surface de ce corps, l'écoulement de phase dispersante à la surface du corps poreux permet l'entraînement des gouttes. L'énergie transmise à l'interface est limitée par les pertes dues aux frottements dans la phase dispersante ; en conséquence les gouttes entraînées sont de taille plus élevée (environ de 4 à 5 fois la taille de pore) et un phénomène de coalescence à la surface du corps poreux se produit augmentant la taille des gouttes et l'inhomogénéité des populations de gouttes. Le phénomène de coalescence intervient quand au moins deux gouttes formées sur des pores voisins se regroupent pour n'en former qu'une. Une solution a ce dernier phénomène perturbateur est envisagée dans les brevet JP2-214537. Elle consiste en l'ajout d'une irradiation ultrasonore du corps poreux. L'onde générée par un système standard de lavage est transmise par voie fluide. Avec une source ultrasonore de moyenne intensité l'agitation ainsi créée inhibe la coalescence mais avec un énergie plus intense on se retrouve dans une configuration d'une machine de dispersion à ultrasons standard, avec les pertes mécaniques et une inhomogénéité des effets. De façon générale, tous ces dispositifs présentent l'inconvénient plus ou moins prononcé de requérir un apport global d'énergie très important par rapport à l'énergie utile au niveau microscopique (rendement inférieur à 10%). Ceci s'explique par le fait que l'énergie mécanique est transmise par les fluides jusqu'à l'interface, engendrant des pertes par frottement fluide plus de dix fois supérieures à l'énergie utile. Cette déperdition d'énergie se traduit en général par une élévation de température importante, ou un matériel que l'on fait travailler à ses limites pour obtenir des effets satisfaisants. De plus les volumes dans lesquels est apportée l'énergie mécanique sont supérieurs à 10"10 m3 pour des actions sur des volumes utiles (taille de particules en dispersion, cellules...) classiquement de l'ordre de 10" m . Au regard de la différence d'échelle, les dispositifs utilisés ne peuvent assurer l'homogénéité de l'action mécanique, de ses effets et donc du produit obtenu. - EXPOSÉ DE L'INVENTION -The advantage of such systems is to arrive at very high volumetric energies. However, the energy is provided in a very inhomogeneous way and the phenomenon of cavitation is not yet completely described by the theory, which forces in the development of devices and processes to adopt essentially empirical approaches. Another emulsion manufacturing system is the membrane emulsification: the dispersed phase which forms drops on the surface of this body is pushed through a porous body, the dispersant phase flow on the surface of the porous body allows the training of the drops. The energy transmitted to the interface is limited by the losses due to friction in the dispersant phase; as a result the entrained drops are of larger size (approximately 4-5 times the pore size) and a phenomenon of coalescence on the surface of the porous body occurs increasing the size of the drops and the inhomogeneity of the droplet populations. The phenomenon of coalescence occurs when at least two drops formed on neighboring pores combine to form one. A solution to this last disturbing phenomenon is envisaged in the JP2-214537 patent. It consists of the addition of an ultrasonic irradiation of the porous body. The wave generated by a standard washing system is transmitted in a fluid way. With an ultrasonic source of medium intensity the stirring thus created inhibits coalescence but with a more intense energy is found in a configuration of a standard ultrasonic dispersion machine, with mechanical losses and inhomogeneity of effects. In general, all these devices have the disadvantage of more or less pronounced require a very large energy input compared to useful energy at the microscopic level (less than 10% efficiency). This is explained by the fact that the mechanical energy is transmitted by the fluids to the interface, generating losses by fluid friction more than ten times higher than the useful energy. This loss of energy generally results in a significant rise in temperature, or a material that is made to work at its limits to obtain satisfactory effects. More volumes in which mechanical energy is supplied are greater than 10 "10 m 3 for actions on useful volumes (particle size in dispersion, cells ...) typically of the order of 10" m. In view of the difference in scale, the devices used can not ensure the homogeneity of the mechanical action, its effects and therefore the product obtained. - PRESENTATION OF THE INVENTION -
L'invention a pour but de proposer un procédé de fabrication d'une dispersion ou d'une emulsion d'au moins deux fluides réputés non miscibles qui évite les inconvénients précités et qui permette la fabrication d'une emulsion ou d'une dispersion homogène à gouttes fines.The purpose of the invention is to propose a process for manufacturing a dispersion or an emulsion of at least two fluids that are considered immiscible, which avoids the aforementioned drawbacks and allows the manufacture of a homogeneous emulsion or dispersion. with fine drops.
L'invention a aussi pour but de proposer un dispositif mettant en œuvre ce procédé, en exerçant une action mécanique directement à l'interface des deux phases, ce qui permet d'obtenir des dispersions plus fines et plus homogènes avec un meilleur rendement énergétique.The object of the invention is also to propose a device implementing this method, by exerting a mechanical action directly at the interface of the two phases, which makes it possible to obtain finer and more homogeneous dispersions with better energy efficiency.
A cet effet, l'invention a pour objet un procédé de fabrication d'une dispersion ou d'une emulsion à partir d'au moins deux fluides réputés non miscibles constituant une phase dispersée et une phase dispersante, la phase dispersée étant poussé à travers un corps poreux dans la phase dispersante, caractérisé en ce que ledit corps poreux est mis en vibration par une excitation de nature mécanique, électrique ou magnétique.For this purpose, the subject of the invention is a process for producing a dispersion or an emulsion from at least two known immiscible fluids constituting a dispersed phase and a dispersant phase, the dispersed phase being pushed through a porous body in the dispersing phase, characterized in that said porous body is vibrated by an excitation of mechanical, electrical or magnetic nature.
De préférence, la phase dispersante circule à la surface de sortie du corps poreux. Selon une variante du procédé, l'on fait re-circuler Pémulsion dans le corps poreux qui se charge en phase dispersée au cours du processus.Preferably, the dispersant phase flows to the exit surface of the porous body. According to a variant of the process, the emulsion is re-circulated in the porous body which is charged in dispersed phase during the process.
De manière préférentielle, les fréquences et/ou la puissance des vibrations sont contrôlées. Avantageusement, l'on ajoute un émulsifîant dans au moins l'une des deux phases.Preferably, the frequencies and / or the power of the vibrations are controlled. Advantageously, an emulsifier is added in at least one of the two phases.
De préférence, la phase dispersée est poussée à travers le corps poreux dans des conditions de température, de pression, de débit, de composition et d'agitation contrôlées. Avantageusement, la phase dispersante circule à la surface du corps poreux dans des conditions de température, de pression, de débit, de composition et d'agitation contrôlées.Preferably, the dispersed phase is pushed through the porous body under conditions of controlled temperature, pressure, flow, composition, and agitation. Advantageously, the dispersant phase circulates on the surface of the porous body under conditions of controlled temperature, pressure, flow, composition and agitation.
Dans une autre variante de ce procédé on superpose à l'excitation aux fréquences générant les vibrations du corps poreux, une onde dans les fréquences des micro-ondes entraînant réchauffement du corps poreux. Préférentiellement, le procédé consiste à utiliser ladite dispersion ou emulsion pour fabriquer des produits cosmétiques, dermo- pharmaceutiques ou pharmaceutiques.In another variant of this method is superimposed on the excitation at the frequencies generating the vibrations of the porous body, a wave in the frequencies of microwaves causing heating of the porous body. Preferably, the process consists in using said dispersion or emulsion to produce cosmetic, dermopharmaceutical or pharmaceutical products.
L'invention a également pour objet un dispositif pour la fabrication d'une dispersion ou d'une emulsion à partir d'au moins un fluide comprenant au moins : un corps poreux ayant une partie poreuse au travers de laquelle est apte à être poussée ledit fluide, ledit corps poreux ayant une cavité dite interne, - une enveloppe entourant de manière étanche au moins ladite partie poreuse de façon à définir une cavité dite externe dans laquelle débouche ladite partie poreuse, ledit fluide étant apte à être amené dans ladite cavité externe, caractérisé en ce qu'il comporte un système de mise en vibration du corps poreux Au sens de l'invention, « directement » est utilisé dan_^ sens ou, contrairement à l'art antérieur, les vibrations ne sont pas essentiellement transmises via l'un des fluides.The invention also relates to a device for the manufacture of a dispersion or an emulsion from at least one fluid comprising at least: a porous body having a porous portion through which is able to be pushed said fluid, said porous body having a so-called internal cavity, a casing sealingly surrounding at least said porous portion so as to define a so-called external cavity in which said porous part opens, said fluid being able to be brought into said external cavity, characterized in that it comprises a system for vibrating the porous body For the purposes of the invention, "directly" is used in the sense or, contrary to the prior art, the vibrations are not essentially transmitted via one of the fluids.
Au sens de l'invention, le dispositif peut être appliqué à la fabrication d'une emulsion ou d'une dispersion à partir de deux fluides réputés non miscibles ou à l'homogénéisation d'une emulsion ou d'une dispersion à partir d'un même fluide.Within the meaning of the invention, the device can be applied to the manufacture of an emulsion or a dispersion from two fluids deemed immiscible or homogenization of an emulsion or dispersion from the same fluid.
De préférence le dispositif comprend un système d'alimentation dudit fluide capable de fournir ledit fluide dans la cavité externe dans des conditions de température, de pression, de débit, de composition et d'agitation contrôlées.Preferably the device comprises a supply system for said fluid capable of supplying said fluid in the external cavity under conditions of controlled temperature, pressure, flow, composition and agitation.
Avantageusement le dispositif comprend un système d'alimentation d'un autre fluide capable de fournir cet autre fluide dans ladite cavité interne dans des conditions de température, de pression, de débit, de composition et d'agitation contrôlées.Advantageously, the device comprises a supply system for another fluid capable of supplying this other fluid in said internal cavity under conditions of controlled temperature, pressure, flow, composition and agitation.
De manière préférentielle, le dispositif comprend un système de soutirage permettant l'évacuation, et le stockage ou la transmission de l'émulsion ou de la dispersion vers un autre système ou encore la recirculation de l'émulsion ou de la dispersion. Selon un mode de réalisation, le système de mise en vibration du corps poreux est constitué d'un bobinage relié à une source de courant alternatif entourant l'enveloppe perméable aux ondes magnétiques générées par le bobinage, le corps poreux étant réalisé en matériau magnétostrictif.Preferably, the device comprises a withdrawal system for evacuation, and storage or transmission of the emulsion or dispersion to another system or the recirculation of the emulsion or dispersion. According to one embodiment, the system for vibrating the porous body consists of a winding connected to a source of alternating current surrounding the envelope permeable to the magnetic waves generated by the winding, the porous body being made of magnetostrictive material.
Selon un autre mode de réalisation, le système de mise en vibration du corps poreux est constitué d'un tige conductrice disposée coaxialement au corps poreux, d'une enveloppe conductrice, ladite tige conductrice et ladite enveloppe étant reliées à une source de courant alternatif, le corps poreux étant constitué d'un matériau piézoélectrique.According to another embodiment, the system for vibrating the porous body consists of a conductive rod disposed coaxially with the porous body, a conductive envelope, said conductive rod and said envelope being connected to an alternating current source, the porous body being made of a piezoelectric material.
Préférentiellement, la tige conductrice et/ou la surface du corps poreux sont recouvertes d'un isolant.Preferably, the conductive rod and / or the surface of the porous body are covered with an insulator.
Selon encore un autre mode de réalisation, le système de mise en vibration du corps poreux est constitué de deux transducteurs fixés aux extrémités du corps poreux et reliés à une source de courant alternatif, lesdits transducteurs étant constitués d'un matériau piézoélectrique.According to yet another embodiment, the system for vibrating the porous body consists of two transducers attached to the ends of the porous body and connected to an AC source, said transducers being made of a piezoelectric material.
Avantageusement, chaque transducteur comporte un moyen de support fixé à l'enveloppe comportant un évidement dans lequel est positionnée une extrémité du corps poreux, ledit moyen de support comportant au moins une paire de trous radiaux, chaque paire contenant un élément piézoélectrique dans un trou et un moyen élastique de sollicitation dans l'autre trou de la même paire pour maintenir l'élément piézoélectrique en appui contre le corps poreux, les trous d'une même paire étant diamétralement opposés.Advantageously, each transducer comprises a support means attached to the casing having a recess in which is positioned an end of the porous body, said support means comprising at least one pair of radial holes, each pair containing a piezoelectric element in a hole and elastic biasing means in the other hole of the same pair for holding the piezoelectric element in abutment against the porous body, the holes of the same pair being diametrically opposed.
De manière préférentielle, le moyen de support comporte deux paires de trous, les deux paires de trous étant disposés dans des directions perpendiculaires, et les deux éléments piézoélectriques sont alimentés par des signaux décalés d'un quart de période l'un par rapport à l'autre, et, en association avec les ressorts de précontrainte, engendrent un déplacement du corps poreux selon une trajectoire globalement circulaire.Preferably, the support means comprises two pairs of holes, the two pairs of holes being arranged in perpendicular directions, and the two piezoelectric elements are powered by signals shifted by a quarter of a period relative to one another. and other, and in combination with the prestressing springs, cause a displacement of the porous body in a generally circular path.
- BRÈVE DESCRIPTION DES DESSINS -- BRIEF DESCRIPTION OF THE DRAWINGS -
L'invention sera mieux comprise, et d'autres buts, détails, caractéristiques et avantages de celle-ci apparaîtront plus clairement au cours de la description explicative détaillée qui va suivre, de plusieurs modes de réalisation de l'invention donnés à titre d'exemples purement illustratifs et non limitatifs, en référence aux dessins schématiques annexés.The invention will be better understood, and other objects, details, features and advantages thereof will become more clearly apparent in the following detailed explanatory description of several embodiments of the invention given as examples. purely examples illustrative and non-limiting, with reference to the attached schematic drawings.
Sur ces dessins : la figure 1 représente une coupe longitudinale d'un module contenant le corps poreux et un moyen d'excitation magnétique, et une coupe selon l'axe A- A de ce module ; la figure 2 est une coupe longitudinale d'un module contenant le corps poreux et un moyen d'excitation électrique, et une coupe selon l'axe A-A de ce module ; - la figure 3 est une coupe longitudinale d'un module contenant le corps poreux et un moyen d'excitation mécanique, et une coupe selon l'axe A-A de ce module ; la figure 4 est une représentation schématique d'une mise en oeuvre de l'invention ; - la figure 5 est une représentation schématique d'une mise en œuvre de l'invention avec re-circulation de l'émulsion ou de la dispersion ; la figure 6 est une représentation schématique détaillée du dispositif présenté sur la figure 5 ; - la figure 7 est une coupe longitudinale d'un module contenant le corps poreux et un moyen d'excitation mécanique selon un second mode de réalisation ; la figure 8 est une vue en perspective d'un manchon de raccord ; - la figure 9 est une coupe selon l'axe IX de la figure 7 d'un module contenant le corps poreux et un moyen d'excitation mécanique ; et la figure 10 est un diagramme présentant les résultats de l'exemple d'application. - DESCRIPTION -In these drawings: FIG. 1 represents a longitudinal section of a module containing the porous body and a magnetic excitation means, and a section along the axis A-A of this module; Figure 2 is a longitudinal section of a module containing the porous body and an electrical excitation means, and a section along the axis A-A of this module; - Figure 3 is a longitudinal section of a module containing the porous body and a mechanical excitation means, and a section along the axis A-A of this module; Figure 4 is a schematic representation of an implementation of the invention; - Figure 5 is a schematic representation of an implementation of the invention with re-circulation of the emulsion or dispersion; Figure 6 is a detailed schematic representation of the device shown in Figure 5; FIG. 7 is a longitudinal section of a module containing the porous body and a mechanical excitation means according to a second embodiment; Figure 8 is a perspective view of a coupling sleeve; - Figure 9 is a section along the axis IX of Figure 7 of a module containing the porous body and a mechanical excitation means; and Fig. 10 is a diagram showing the results of the application example. - DESCRIPTION -
Sur les figures 1, 2, 3 et 7 le dispositif se présente sous forme de module actif 2, 102 et 202.In Figures 1, 2, 3 and 7 the device is in the form of active module 2, 102 and 202.
Selon la figure 1, ce module 2 est composé d'un corps poreux 24, d'un bobinage 27 et d'une enveloppe 23. Le corps poreux 24 est sous forme d'un cylindre creux dont la partie poreuse 42 centrale est comprise dans l'enveloppe 23 de forme cylindrique coaxiale au coφs poreux 24. L'espace compris entre le coφs poreux 24 et l'enveloppe 23 définit une cavité externe 21.According to FIG. 1, this module 2 is composed of a porous body 24, a coil 27 and a casing 23. The porous body 24 is in the form of a hollow cylinder whose central porous portion 42 is included in FIGS. the envelope 23 of form cylindrical coaxial with porous coφs 24. The space between the porous coφs 24 and the envelope 23 defines an external cavity 21.
L'enveloppe 23 est reliée aux extrémités 43 du coφs poreux 24 par un système d'étanchéité 25 et 25'. Une cavité interne 22 est également définie à l'intérieur du corps poreux 24.The casing 23 is connected to the ends 43 of the porous coφs 24 by a sealing system 25 and 25 '. An internal cavity 22 is also defined inside the porous body 24.
Le bobinage 27 relié à une source de courant alternatif 4 de puissance et fréquence réglables, produit un champ magnétique oscillant. Le coφs poreux 24 est réalisé dans un matériau magnétostrictif et l'enveloppe 23 dans un matériau perméable aux ondes magnétiques produites par le bobinage 27.The coil 27 connected to a source of alternating current 4 of adjustable power and frequency produces an oscillating magnetic field. The porous coφs 24 is made in a magnetostrictive material and the envelope 23 in a material permeable to the magnetic waves produced by the coil 27.
La phase dispersée 40 est amenée par l' orifice 26 dans la cavité externe 21, puis elle est poussée au travers de la partie poreuse 42 jusqu'à la cavité interne 22, au niveau de la surface dite de sortie où elle sera mise en contact avec la phase dispersante 44 circulant de l'extrémité 43 gauche du coφs poreux vers celle de droite. La mise en contact de la phase dispersée 40 sous forme de gouttelettes après passage au travers de la partie poreuse 42 et de la phase dispersante 44 est à la base de l'émulsion ou de la dispersion 41.The dispersed phase 40 is fed through the orifice 26 into the external cavity 21, then it is pushed through the porous portion 42 to the internal cavity 22, at the so-called outlet surface where it will be placed in contact. with the dispersing phase 44 flowing from the left end 43 of the porous coφs to that of the right. Contacting the dispersed phase 40 in the form of droplets after passing through the porous part 42 and the dispersing phase 44 is at the base of the emulsion or dispersion 41.
L'enveloppe 23 a pour rôle de comporter la phase dispersée 40 qui sera poussée au travers du coφs poreux 24 et permettre les vibrations du coφs poreux 24 sans dégradation de celui-ci.The envelope 23 serves to comprise the dispersed phase 40 which will be pushed through the porous coφs 24 and allow the vibrations of the porous coφs 24 without degradation thereof.
Le système d'étanchéité 25 et 25 'pourra être avantageusement composé de deux joints souples assurant à la fois l'étanchéité et la mobilité du corps poreux par rapport à l'enveloppe 23. Le mode de réalisation représenté sur la figure 1 est un système de mise en vibration 51 par excitation magnétique c'est-à-dire que le système 51 est composé de la source de courant alternatif 4 reliée au bobinage 27 dont la géométrie permet d'exercer sur le coφs poreux 24 un champ magnétique alternatif. Le corps poreux 24 ainsi soumis à un champ magnétique oscillant vibre et exerce sur l'interface des deux phases 40 et 44, l'action mécanique recherchée. Par cette action mécanique produite à l'interface des phases 40 et 44, les gouttelettes ainsi formées sont séparées rapidement du pore d'où elles proviennent et se mélangent à la phase dispersante 44 avec une taille de gouttelette très petite. Le mode de réalisation représenté sur la figure 2, illustre un système de mise en vibration 151 par excitation électrique.The sealing system 25 and 25 'may advantageously be composed of two flexible joints ensuring both the sealing and the mobility of the porous body with respect to the envelope 23. The embodiment shown in FIG. of vibrating 51 by magnetic excitation that is to say that the system 51 is composed of the alternating current source 4 connected to the coil 27 whose geometry makes it possible to exert on the porous coφs 24 an alternating magnetic field. The porous body 24 thus subjected to an oscillating magnetic field vibrates and exerts on the interface of the two phases 40 and 44, the desired mechanical action. By this mechanical action produced at the interface of the phases 40 and 44, the droplets thus formed are rapidly separated from the pore from which they originate and mix with the dispersant phase 44 with a very small droplet size. The embodiment shown in FIG. 2 illustrates a vibrating system 151 by electrical excitation.
Les éléments identiques porteront les mêmes références et ne seront pas à nouveau décrits. Le module actif 102 diffère de celui présenté sur la figure 1 seulement par le système de mise en vibration.The identical elements will bear the same references and will not be described again. The active module 102 differs from that shown in FIG. 1 only by the vibrating system.
Le système de mise en vibration 151 comprend alors une source de courant alternatif 4 reliée à des surfaces conductrices entre lesquelles on place le coφs poreux 24. Les surfaces conductrices sont constituées par la couche conductrice 46 de l'enveloppe 23 et une tige conductrice 28 placée coaxialement au cylindre formé par le coφs poreux 24. Chacune des surfaces conductrices 46 et 28 est reliée à une borne d'une source de courant alternatif 4 de puissance et fréquence réglables créant un champ électrique oscillant.The vibrating system 151 then comprises an alternating current source 4 connected to conductive surfaces between which the porous coφs 24 is placed. The conductive surfaces consist of the conductive layer 46 of the envelope 23 and a conducting rod 28 placed coaxially with the cylinder formed by the porous coφs 24. Each of the conductive surfaces 46 and 28 is connected to a terminal of an alternating current source 4 of adjustable power and frequency creating an oscillating electric field.
La tige conductrice 28 est réalisée dans un matériau conducteur avantageusement recouvert d'une couche isolante 45, de même que l'enveloppe 23 comprend au moins une couche conductrice 46 avantageusement recouverte d'un isolant 47 (représenté par le trait noir épais définissant le contour de la cavité externe 21).The conducting rod 28 is made of a conductive material advantageously covered with an insulating layer 45, just as the envelope 23 comprises at least one conductive layer 46 advantageously covered with an insulator 47 (represented by the thick black line defining the outline of the external cavity 21).
Le coφs poreux 24 réalisé dans un matériau piézo-électrique et soumis à ce champ, vibre et exerce ainsi à l'interface des phases dispersée 40 et dispersante 44, l'action mécanique recherchée.The porous coφs 24 made in a piezoelectric material and subjected to this field, vibrates and thus exerts at the interface of dispersed phases 40 and dispersant 44, the desired mechanical action.
Le mode de réalisation représenté sur la figure 3, illustre un système de mise en vibration 251 par excitation mécanique.The embodiment shown in FIG. 3 illustrates a mechanical excitation vibration system 251.
Les éléments identiques porteront les mêmes références et ne seront pas à nouveau décrits.The identical elements will bear the same references and will not be described again.
Le module actif 202 diffère de celui présenté sur les figures 1 et 2 seulement par le système de mise en vibration. Le système de mise en vibration 251 comprend alors une source de courant alternatif 4 et 4' reliée à un ou plusieurs vibrateurs mécaniques couplés (liaison mécanique) avec le coφs poreux 24, pouvant être avantageusement des transducteurs 29 et 29' en forme de collier fixés aux extrémités 43 du coφs poreux 24. Ces transducteurs 29 et 29' transmettent directement les vibrations au coφs poreux 24. Dans ce cas, le système formé par les transducteurs 29 et 29' et le coφs poreux 24 forme un oscillateur exerçant ainsi à l'interface des phases dispersée 40 et dispersante 44, l'action mécanique recherchée.The active module 202 differs from that shown in Figures 1 and 2 only by the vibrating system. The vibrating system 251 then comprises an alternating current source 4 and 4 'connected to one or more coupled mechanical vibrators (mechanical connection) with the porous coφs 24, which may advantageously be fixed collar-shaped transducers 29 and 29' at the ends 43 of the porous coφs 24. These transducers 29 and 29 'directly transmit the vibrations to the porous coφs 24. In this case, the system formed by the transducers 29 and 29 'and the porous coφs 24 forms an oscillator thus exerting the desired mechanical action at the dispersed phase 40 and dispersant 44 interface.
Un mode de réalisation particulier des transducteurs 290 et 290' en forme de collier est représenté sur les figures 7 et 9.A particular embodiment of the transducers 290 and 290 'in the form of a collar is shown in FIGS. 7 and 9.
D'après la figure 7, les transducteurs 290 et 290' sont placés au niveau de chaque extrémité 43 du coφs poreux 24 de manière fixe contre l'enveloppe 23 et le système d'étanchéité 25 et 25'.According to Figure 7, the transducers 290 and 290 'are placed at each end 43 of the porous coφs 24 fixedly against the casing 23 and the sealing system 25 and 25'.
Les transducteurs 290 et 290 'sont formés d'un moyen de support 291 et 291' par exemple sous forme de collier octogonal comportant un évidement 52 coaxial à l'axe X et selon la figure 9, deux trous taraudés radiaux 293a et 293b. L'extrémité 43 du coφs poreux 24 est emboîtée dans un manchon de raccord 292 ou 292' lui même placé dans l'évidement coaxial 52. Ce manchon de raccord 292, d'après la figure 8 est une pièce façonnée composée d'un cylindre creux traversant un cube de largeur supérieure au diamètre externe du cylindre au niveau de sa portion médiane c'est à dire qu'au niveau de la portion médiane du manchon 292, la section se présente sous la forme d'un carré évidé d'un cercle correspondant au diamètre interne du cylindre. L'extrémité 43 du coφs poreux 24 est placée de manière fixe dans le manchon 292 de manière que le manchon 292 transmette le mouvement qui lui est appliqué au coφs poreux 24.The transducers 290 and 290 'are formed of a support means 291 and 291' for example in the form of an octagonal collar having a recess 52 coaxial with the X axis and according to Figure 9, two radial tapped holes 293a and 293b. The end 43 of the porous coφs 24 is nested in a connecting sleeve 292 or 292 'itself placed in the coaxial recess 52. This coupling sleeve 292, according to FIG. 8, is a shaped part composed of a cylinder hollow traversing a cube of greater width than the outer diameter of the cylinder at its median portion, that is to say that at the middle portion of the sleeve 292, the section is in the form of a hollow square of a circle corresponding to the internal diameter of the cylinder. The end 43 of the porous coφs 24 is fixedly placed in the sleeve 292 so that the sleeve 292 transmits the movement applied to it to the porous coφs 24.
Selon la figure 9, dans chaque trou 293a et 293b est placé un élément piézo-électrique 294 et un ressort de précontrainte 295 de part et d'autre du manchon de raccord 292. Quatre vis de réglage 296a, 296b, 296c et 296d obturent les extrémités de chaque trou 293a et 293b. Les ressorts de précontrainte 295 sont précontraints en compression au moyen des quatre vis 296a, 296b, 296c et 296d précitées. Les éléments piézo-électriques 294 sont alimentés par deux signaux électriques périodiques en quadrature l'un par rapport à l'autre (i.e. : décalage d'un quart de période) et subissent une élongation proportionnelle à la tension d'alimentation. Ils agissent en traction et en compression peφendiculairement à l'axe du coφs poreux 24 générant ainsi des modes de vibration des extrémités 43 du coφs poreux 24 entraînant sa flexion. Comme le signal d 'entrée est rarement pur, c'est à dire qu'il comporte en outre le signal principal à une fréquence donnée, d'autres signaux secondaires à d'autres fréquences, les mouvements alors décrits par les sections transversales du coφs poreux 24 sont composés d'une somme de trajectoires circulaires (correspondant chacune à une fréquence du signal d'entrée), garantissant sur une section une trajectoire globale circulaire. En outre, les deux signaux d'entrée sur les deux éléments piézoélectriques sont identiques au quart de période près, pour assurer que chaque point du corps poreux 24 au niveau d'une section transversale donnée subisse les mêmes vibrations et garantir ainsi une homogénéité d'action mécanique.According to FIG. 9, in each hole 293a and 293b is placed a piezoelectric element 294 and a prestressing spring 295 on either side of the connecting sleeve 292. Four adjustment screws 296a, 296b, 296c and 296d close off the ends of each hole 293a and 293b. The prestressing springs 295 are prestressed in compression by means of the four screws 296a, 296b, 296c and 296d mentioned above. The piezoelectric elements 294 are powered by two periodic electric signals in quadrature with respect to each other (ie: shift of a quarter period) and undergo an elongation proportional to the supply voltage. They act in tension and in compression peφendiculairement to the axis of the porous coφs 24 thus generating modes of vibration of the ends 43 of the porous coφs 24 causing its flexion. Since the input signal is rarely pure, it is up to say that it further comprises the main signal at a given frequency, other signals secondary to other frequencies, the movements then described by the transverse sections of the porous coφs 24 are composed of a sum of circular trajectories (corresponding each at a frequency of the input signal), guaranteeing on a section a global circular trajectory. In addition, the two input signals on the two piezoelectric elements are identical to the nearest quarter of a period, to ensure that each point of the porous body 24 at a given cross-section undergoes the same vibrations and thus guarantee homogeneity of mechanical action.
Les transducteurs 290 et 290' sont alimentés par des signaux de fréquences distinctes correspondant chacun à un mode propre du système. Ceci permet une optimisation et un bon contrôle de la génération des vibrations, tout en évitant les nœuds de vibration où l'action mécanique serait absente.The transducers 290 and 290 'are powered by separate frequency signals each corresponding to a specific mode of the system. This allows an optimization and a good control of the generation of the vibrations, while avoiding the nodes of vibration where the mechanical action would be absent.
Dans le mode de mise en œuvre de l'invention représenté sur la figure 4, le dispositif comprend un module actif 2 relié par la canalisation 5 au système d'alimentation 1 en phase dispersée 40, par la canalisation 7 au système d'alimentation 8 en phase dispersante 44 et par la canalisation 6 au système de soutirage 3. Le module actif 2 est également relié à une source de courant alternatif 4.In the embodiment of the invention shown in FIG. 4, the device comprises an active module 2 connected by the pipe 5 to the supply system 1 in dispersed phase 40, via the pipe 7 to the supply system 8 in the dispersing phase 44 and through the pipe 6 to the withdrawal system 3. The active module 2 is also connected to an alternating current source 4.
La source de courant alternatif 4 apporte au module actif 2 l'énergie nécessaire à la génération de l'action mécanique nécessaire à la génération de fines gouttelettes. Le système de soutirage 3, relié au module actif 2 par la canalisation 6 permet l'évacuation de l'émulsion ou de la dispersion 41 du coφs poreux 24.The AC source 4 supplies the active module 2 with the energy necessary to generate the mechanical action necessary for the generation of fine droplets. The withdrawal system 3 connected to the active module 2 via the pipe 6 allows the evacuation of the emulsion or dispersion 41 of the porous coφs 24.
Une variante de cette mise en œuvre, représentée sur la figure 5 comprend les mêmes éléments que dans le mode de mise en œuvre précédent à part qu'une canalisation 17 relie le système de soutirage 3 au module 2. Le système de soutirage 3 permet alors le retour de l'émulsion ou de la dispersion 41, créant ainsi une re-circulation.A variant of this implementation, shown in FIG. 5, comprises the same elements as in the previous embodiment, except that a pipe 17 connects the withdrawal system 3 to the module 2. The withdrawal system 3 then allows the return of the emulsion or dispersion 41, thus creating a recirculation.
Selon la figure 6, dans cette variante de mise en oeuvre le système de soutirage 3, est composé d'au moins un réservoir 30 et d'une pompe 33 située entre ce réservoir 30 et la canalisation 17. Le réservoir 30 est muni d'un système d'agitation 31 et d'un système de maintien de la température 50 composé d'un bain thermostaté 35 et d'une spire échangeuse 34.According to FIG. 6, in this alternative embodiment the draw-off system 3 is composed of at least one tank 30 and a pump 33 located between this tank 30 and the pipe 17. The tank 30 is provided with a stirring system 31 and a system for maintaining the temperature 50 composed of a thermostated bath 35 and an exchange coil 34.
Le système d'alimentation 1 en phase dispersée 40 comprend une alimentation 48 en gaz sous pression composée d'un réservoir 13 (bouteille sous pression, ou compresseur couplé à un vase d'expansion) et d'un détendeur 14. Le système 1 comprend également un réservoir 10 de phase dispersée 40, pressurisable, muni d'un système d'agitation 11, et monté sur un peson ou une balance 15. Le système 1 comprend enfin une vanne de sectionnement 12. Le détendeur 14 permet de fixer la pression à laquelle est poussée la phase dispersée 40 au niveau du système d'alimentation 1.The disperse phase feed system 40 comprises a feed 48 of pressurized gas composed of a reservoir 13 (pressurized bottle, or compressor coupled to an expansion vessel) and a pressure reducer 14. The system 1 comprises also a disperse phase reservoir 40, pressurizable, provided with a stirring system 11, and mounted on a scale or balance 15. The system 1 finally comprises a shutoff valve 12. The pressure regulator 14 can set the pressure to which is pushed the dispersed phase 40 at the level of the feed system 1.
Le peson ou une balance 15 sont utilisés pour contrôler la masse et le flux de phase dispersée 40 injectée dans le système d'alimentation 1. - EXEMPLE D'APPLICATION -The scale or balance is used to control the mass and the flow of dispersed phase injected into the feed system 1. EXAMPLE OF APPLICATION
Un mode de réalisation de l'invention est maintenant décrit à titre d'exemple non limitatif.An embodiment of the invention is now described by way of non-limiting example.
Le module actif utilisé correspond à celui représenté sur la figure 3 avec un mode de réalisation identique à celui de la figure 6. Le module actif peut être avantageusement un module de filtration tangentielle monocanal adapté à l'application, utilisant des coφs poreux en céramique hydrophile de diamètre de pore 0,1 μm et 0,8 μm. Un coφs poreux cylindrique creux de longueur entre 20 et 30 mm et de rayon extérieur entre 10 et 15 mm et de rayon intérieur entre 7 et 12 mm sera utilisé.The active module used corresponds to that shown in FIG. 3 with an embodiment identical to that of FIG. 6. The active module can advantageously be a single-channel tangential filtration module adapted to the application, using porous coφs made of hydrophilic ceramic. with a pore diameter of 0.1 μm and 0.8 μm. A hollow cylindrical porous coφs of length between 20 and 30 mm and outer radius between 10 and 15 mm and inner radius between 7 and 12 mm will be used.
L'exemple de réalisation concerne la fabrication d'une emulsion 41 de type huile dans l'eau, composée par exemple de 10 % d'huile de soja, 0,5 % d'émulsifïant Tween 20 (marque déposée) et 89,5 % d'eau. Un mélange de 4,8 % de Tween 20 et 95,2 % d'huile est réalisé dans le réservoir 10 sous agitation. Puis une quantité d'eau X est mise en circulation à partir du réservoir 30. Une fois la vanne 12 fermée, le détendeur 14 est réglé sur une pression entre 0,1 et 5 bars. Les transducteurs 29 et 29' sont alimentés indépendamment avec la source de courant alternatif 4 (composée de deux sources séparées) avec des signaux de puissances comprises entre 0 W et 2 kW et de deux fréquences dont une est comprise entre 14 et 16 kHz et la deuxième entre 18 et 22 kHz. Puis la vanne 12 est ouverte et refermée lorsque la quantité de mélange huile + émulsifiant atteint 0,1173X. Durant toute l'opération, la température est maintenue autour d'une température de consigne comprise entre 15 et 25°C.The exemplary embodiment relates to the manufacture of an emulsion 41 of the oil-in-water type, composed for example of 10% of soybean oil, 0.5% of Tween 20 (registered trademark) and 89.5 emulsifier. % of water. A mixture of 4.8% Tween 20 and 95.2% oil is made in the tank 10 with stirring. Then a quantity of water X is circulated from the tank 30. Once the valve 12 is closed, the expander 14 is set to a pressure between 0.1 and 5 bar. The transducers 29 and 29 'are independently powered with the AC source 4 (composed of two separate sources) with power signals between 0 W and 2 kW and two frequencies one of which is between 14 and 16 kHz and the second between 18 and 22 kHz. Then the valve 12 is opened and closed when the amount of oil + emulsifier mixture reaches 0,1173X. During the entire operation, the temperature is maintained around a set temperature of between 15 and 25 ° C.
Afin de vérifier l'apport des vibrations dans l'effet technique recherché, la même expérience est réalisée sans vibration. Puis les répartitions volumiques des tailles de gouttes des émulsions obtenues avec ou sans vibrations sont mesurées par un granulomètre à diffraction laser Malvern (marque déposée). Les résultats des mesures pour un coφs poreux 24 de taille de pores de 0,8 μm avec et sans vibrations générées par une puissance de 50 W sont illustrés sur la figure 10, diagramme présentant le pourcentage volumique des populations de gouttes en fonction de leur taille (en échelle logarithmique). La répartition des populations est représentée par un trait interrompu pour l'essai sans vibration et avec un trait continu pour l'essai avec vibrations. On constate dans chaque cas la présence de plusieurs populations de gouttes, identifiées par plusieurs pics. La présence de ces mêmes populations de gouttes a été confirmée par des images prises avec un microscope électronique (images non représentées).In order to verify the contribution of the vibrations in the desired technical effect, the same experiment is carried out without vibration. Then, the volume distributions of the drop sizes of the emulsions obtained with or without vibrations are measured by a Malvern (trademark) laser diffraction granulometer. The results of the measurements for a porous coφs of pore size 0.8 μm with and without vibrations generated by a power of 50 W are illustrated in FIG. 10, diagram presenting the percentage by volume of the droplet populations according to their size. (in logarithmic scale). The population distribution is represented by a broken line for the vibration-free test and a continuous line for the vibration test. In each case, we can observe the presence of several droplet populations, identified by several peaks. The presence of these same populations of drops has been confirmed by images taken with an electron microscope (images not shown).
Une grande proportion de population de taille élevée est observée dans le cas où aucune vibration n'est appliquée (plus de 15 % volumique) et semble être due au phénomène de coalescence. En outre une nette diminution de cette proportion est observée (environ 12 % volumique) avec l'utilisation de vibrations. Ainsi l'utilisation des vibrations semble inhiber la coalescence. On constate aussi un décalage des pics vers des valeurs de taille plus faible (de 30 μm pour les essais sans vibration et 10 μm pour les essais avec vibrations) ce qui semble indiquer que les vibrations facilitent la formation et l'arrachement des gouttes. Il semble également que les vibrations facilitent le flux de phase dispersée à travers le coφs poreux 24 car des écarts de 10 % ont été constatés lors des essais. Ces hypothèses ne doivent, néanmoins, aucunement être considérées comme limitatives de l'invention.A large proportion of large population is observed in the case where no vibration is applied (more than 15% volumic) and seems to be due to the coalescence phenomenon. In addition, a clear decrease in this proportion is observed (about 12% by volume) with the use of vibrations. Thus the use of vibrations seems to inhibit coalescence. There is also a shift of the peaks towards values of smaller size (of 30 microns for the tests without vibration and 10 microns for the tests with vibrations) what seems to indicate that the vibrations facilitate the formation and the tearing of the drops. It also seems that the vibrations facilitate the flow of phase dispersed through the porous coφs 24 because deviations of 10% were observed during the tests. These hypotheses must, however, in no way be considered as limiting the invention.
En outre avec une puissance électrique de 200 W et un coφs poreux 24 de diamètre de pore de 0,1 μm, une emulsion 41 dont la taille de goutte est inférieure à 300 nm est obtenue (résultats non représentés). II peut être intéressant d'appliquer cet exemple notamment à la fabrication de produits cosmétiques, dermo-pharmaceutiques ou pharmaceutiques.In addition, with an electric power of 200 W and a porous coφs 24 with a pore diameter of 0.1 μm, an emulsion 41 whose drop size is less than 300 nm is obtained (results not shown). It may be advantageous to apply this example in particular to the manufacture of cosmetic, dermo-pharmaceutical or pharmaceutical products.
Dans la description détaillée des dessins qui précède, l'on aura distingué trois systèmes de mise en vibration du coφs poreux : par excitation mécanique 251 , électrique 151 ou magnétique 51. Ces divers systèmes 51 , 151 et 251 sont susceptibles d'être couplés pour un effet optimal. Il faut également noter que, dans le cas des excitations magnétiques et électriques, les deux principes ont été distingués. Cependant la génération d'un champ magnétique oscillant entraîne selon les équations de Maxwell la génération d'un champ électrique oscillant (et inversement), couplant de fait les deux effets.In the detailed description of the preceding drawings, three systems of vibration of the porous coφs have been distinguished: by mechanical excitation 251, electrical 151 or magnetic 51. These various systems 51, 151 and 251 are capable of being coupled to each other. an optimal effect. It should also be noted that in the case of magnetic and electrical excitations, the two principles have been distinguished. However, the generation of an oscillating magnetic field drives, according to Maxwell's equations, the generation of an oscillating electric field (and vice versa), effectively coupling the two effects.
Les vibrations de la surface de sortie du coφs poreux 24 agissent dans cette invention, libérant une énergie mécanique de rupture directement à l'interface des phases dispersée 40 et dispersante 44, permettant d'éviter la formation de grosses gouttes et générant la formation de fines gouttes de phase dispersée 40 dans la phase dispersante 44 à la base de l'émulsion 41.The vibrations of the exit surface of the porous coφs 24 act in this invention, releasing a mechanical energy of rupture directly at the dispersed and dispersive phase interface 44, making it possible to avoid the formation of large drops and generating the formation of fines. drops of dispersed phase 40 in the dispersing phase 44 at the base of the emulsion 41.
Le système permet ainsi de transmettre à l'interface des deux phases 40 et 44 une énergie importante ; la transmission se faisant par un solide (le coφs poreux 24) et non par les fluides. Il semble que dans ces conditions les phénomènes de coalescence soient inhibés, et le mécanisme de formation et d'arrachement des gouttes accéléré. Cette hypothèse ne doit, néanmoins, aucunement être considérée comme limitative de l'invention.The system thus makes it possible to transmit at the interface of the two phases 40 and 44 a large amount of energy; the transmission being done by a solid (the porous coφs 24) and not by the fluids. It seems that under these conditions the phenomena of coalescence are inhibited, and the mechanism of formation and tearing drops accelerated. This hypothesis must, however, in no way be considered as limiting the invention.
Le choix du mode de mise en vibration impose des propriétés magnétostrictives, piézoélectriques ou electrostrictives au coφs poreux. D'autres propriétés, géométriques, mécaniques, physico-chimiques, chimiques sont déterminées par l'application. La forme générale du coφs poreux 24 doit permettre d'optimiser la surface au travers de laquelle passe la phase dispersée 40 tout en facilitant la transmission ou la génération de vibrations. L'une de ces formes, le cylindre creux (on reprend alors le principe de montage de membrane de filtration tangentielle), est celle qui a été présentée précédemment. On peut citer également à titre d'exemple un cylindre plein placé dans une canalisation la phase dispersée s 'écoulant selon l'axe du cylindre, ou encore un bouchon fixé dans une canalisation, et dont la surface de sortie affleure la surface intérieure d'une cuve agitée. La porosité, la taille de pores et l'épaisseur du coφs poreux 24 déterminent le volume efficace, et la durée de l'action mécanique. La résistance mécanique et l'élasticité jouent sur l'amplitude des vibrations et donc l'intensité de l'action mécanique. Le caractère hydrophile / hydrophobe peut modifier sensiblement les trajets du fluide au travers du coφs mais également l'interface coφs poreux 24 // phase dispersée 40 // phase dispersante 44 (angle de contact). On choisit alors avantageusement un coφs 24 ayant une bonne affinité avec la phase dispersante 44 afin de favoriser le décollement des gouttes de phase dispersée 40. Il faut également que les matériaux choisis soient compatibles avec les produits utilisés. En utilisant un coφs non perméable aux micro-ondes il est impossible de chauffer ce coφs et d'ajouter à l'effet mécanique un effet thermique.The choice of the vibrating mode imposes magnetostrictive, piezoelectric or electrostrictive properties at the porous coφs. Other properties, geometric, mechanical, physico-chemical, chemical are determined by the application. The general shape of the porous coφs 24 must optimize the surface through which the dispersed phase 40 passes while facilitating the transmission or generation of vibrations. One of these forms, the hollow cylinder (we then take the principle of tangential filtration membrane assembly), is the one that has been presented previously. By way of example, a solid cylinder placed in a pipe may also be mentioned, the dispersed phase flowing in accordance with the axis of the cylinder, or a plug fixed in a pipe, and whose outlet surface is flush with the inner surface of a stirred tank. The porosity, the pore size and the thickness of the porous coφs 24 determine the effective volume, and the duration of the mechanical action. The mechanical resistance and the elasticity play on the amplitude of the vibrations and thus the intensity of the mechanical action. The hydrophilic / hydrophobic character can substantially modify the fluid paths through the coφs but also the porous coφs interface 24 // dispersed phase 40 // dispersant phase 44 (contact angle). A coφs 24 having a good affinity with the dispersing phase 44 is thus advantageously chosen in order to favor the separation of the drops of disperse phase 40. It is also necessary that the chosen materials be compatible with the products used. By using a coφs not permeable to microwaves it is impossible to heat this coφs and add to the mechanical effect a thermal effect.
De façon générale on note que le coφs poreux 24 n'est pas nécessairement homogène. A titre d'exemple on peut choisir un coφs poreux 24 dont seule la couche au contact de la phase dispersante 44 possède une porosité adaptée, le reste du coφs 24 servant de support à cette couche. De même, pour garantir l'étanchéité nécessaire au passage imposé de la phase dispersée 40 à travers le coφs poreux 24, une partie du coφs 24 située à ses extrémités 43 peut être non poreuse. Ainsi on définit les propriétés du coφs poreux 24 et par suite sa composition et son traitement, en fonction de l'application. Bien que l'invention ait été décrite en relation avec plusieurs modes de réalisation particuliers, il est bien évident qu'elle n'y est nullement limitée et qu'elle comprend tous les équivalents techniques des moyens décrits ainsi que leurs combinaisons si celles-ci entrent dans le cadre de l'invention. In general, it should be noted that the porous coφs 24 is not necessarily homogeneous. By way of example, it is possible to choose a porous coφs 24 of which only the layer in contact with the dispersing phase 44 has a suitable porosity, the remainder of the coφs 24 serving to support this layer. Similarly, in order to guarantee the tightness necessary for the imposed passage of the dispersed phase 40 through the porous coφs 24, a part of the coφs 24 located at its ends 43 may be non-porous. Thus one defines the properties of the porous coφs 24 and consequently its composition and its treatment, according to the application. Although the invention has been described in connection with several particular embodiments, it is obvious that it is not limited thereto and that it comprises all the technical equivalents of the means described and their combinations if they are within the scope of the invention.

Claims

REVENDICATION CLAIM
1) Procédé de fabrication d'une dispersion ou d'une emulsion (41) à partir d'au moins deux fluides réputés non miscibles, lesdits fluides constituant une phase dispersée (40) et une phase dispersante (44), ladite phase dispersée (40) étant poussée à travers un coφs poreux (24) dans la phase dispersante (44), caractérisé en ce que ledit coφs poreux (24) est mis en vibration par une excitation de nature mécanique, électrique ou magnétique.1) Process for producing a dispersion or an emulsion (41) from at least two fluids that are considered immiscible, said fluids constituting a dispersed phase (40) and a dispersing phase (44), said dispersed phase ( 40) being pushed through a porous coφs (24) into the dispersing phase (44), characterized in that said porous coφs (24) is vibrated by an excitation of mechanical, electrical or magnetic nature.
2) Procédé selon la revendication 1, caractérisé en ce que la phase dispersante (44) circule à la surface de sortie du coφs poreux (24).2) Process according to claim 1, characterized in that the dispersing phase (44) flows at the exit surface of the porous coφs (24).
3) Procédé selon la revendication 2, caractérisé en ce que l'on fait re-circuler l'émulsion (41) dans le coφs poreux (24) qui se charge en phase dispersée (40) au cours du processus.3) Process according to claim 2, characterized in that it is made to circulate the emulsion (41) in the porous coφs (24) which loads in the dispersed phase (40) during the process.
4) Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les fréquences et/ou la puissance des vibrations sont contrôlées.4) Method according to any one of the preceding claims, characterized in that the frequencies and / or the power of the vibrations are controlled.
5) Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'on ajoute un émulsifiant dans au moins l'une des deux phases (40, 44). 6) Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la phase dispersée (40) est poussée à travers le coφs poreux (24) dans des conditions de température, de pression, de débit, de composition et d'agitation contrôlées.5) Process according to any one of the preceding claims, characterized in that an emulsifier is added in at least one of the two phases (40, 44). 6) Process according to any one of the preceding claims, characterized in that the dispersed phase (40) is pushed through the porous coφs (24) under conditions of temperature, pressure, flow, composition and stirring controlled.
7) Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la phase dispersante (44) circule à la surface du coφs poreux (24) dans des conditions de température, de pression, de débit, de composition, et d'agitation contrôlées.7) Process according to any one of the preceding claims, characterized in that the dispersing phase (44) flows on the surface of the porous coφs (24) under conditions of temperature, pressure, flow, composition, and controlled agitation.
8) Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'on supeφose à l'excitation aux fréquences générant les vibrations du coφs poreux, une onde dans les fréquences des micro-ondes entraînant l'échauf ement du coφs poreux (24).8) Process according to any one of the preceding claims, characterized in that it is supeφose excitation at the frequencies generating the vibrations of the porous coφs, a wave in the microwave frequencies causing the heating of porous coφs (24).
9) Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'il consiste à utiliser ladite dispersion ou emulsion (41) pour fabriquer des produits cosmétiques, dermo- pharmaceutiques ou pharmaceutiques. 10) Dispositif pour la fabrication d'une dispersion ou d'une emulsion (41) à partir d'au moins un fluide, comprenant au moins : un coφs poreux (24) ayant une partie poreuse (42) au travers de laquelle est apte à être poussée ledit fluide (40), ledit coφs poreux (24) ayant une cavité dite interne (22), une enveloppe (23) entourant de manière étanche au moins ladite partie poreuse (42) de façon à définir une cavité dite externe (21) dans laquelle débouche ladite partie poreuse (42), ledit fluide (40) étant apte à être amené dans ladite cavité externe (21), caractérisé en ce qu'il comporte un système de mise en vibration (51, 151, 251) du coφs poreux (24) pour appliquer directement des vibrations au coφs poreux (24).9) Process according to any one of the preceding claims, characterized in that it consists in using said dispersion or emulsion (41) to manufacture cosmetic, dermopharmaceutical or pharmaceutical products. 10) Device for the manufacture of a dispersion or an emulsion (41) from at least one fluid, comprising at least: a porous coφs (24) having a porous part (42) through which is suitable to be pushed said fluid (40), said porous coφs (24) having a so-called internal cavity (22), an envelope (23) sealingly surrounding at least said porous portion (42) so as to define a so-called external cavity ( 21) into which said porous part (42) opens, said fluid (40) being adapted to be brought into said external cavity (21), characterized in that it comprises a vibrating system (51, 151, 251) porous coφs (24) for directly applying vibrations to the porous coφs (24).
11) Dispositif selon la revendication 10, caractérisé en ce qu'il comprend un système d'alimentation (1) dudit fluide (40) capable de fournir ledit fluide (40) dans la cavité externe (21) dans des conditions de température, de pression, de débit, de composition et d'agitation contrôlées.11) Device according to claim 10, characterized in that it comprises a supply system (1) of said fluid (40) capable of supplying said fluid (40) in the external cavity (21) under conditions of temperature, controlled pressure, flow rate, composition and agitation.
12) Dispositif selon l'une quelconque des revendications 10 ou 11, caractérisé en ce qu'il comprend un système d'alimentation (8) d'un autre fluide (44) capable de fournir cet autre fluide (44) dans ladite cavité interne (22) dans des conditions de température, de pression, de débit, de composition et d'agitation contrôlées.12) Device according to any one of claims 10 or 11, characterized in that it comprises a supply system (8) of another fluid (44) capable of supplying the other fluid (44) in said internal cavity (22) under conditions of controlled temperature, pressure, flow, composition and agitation.
13) Dispositif selon l'une quelconque des revendications 10, 11 ou 12, caractérisé en ce qu'il comprend un système de soutirage (3) permettant l'évacuation, et le stockage ou la transmission de l'émulsion ou de la dispersion (41) vers un autre système ou encore la re-circulation de l'émulsion ou de la dispersion (41).13) Device according to any one of claims 10, 11 or 12, characterized in that it comprises a withdrawal system (3) for the evacuation, and storage or transmission of the emulsion or dispersion ( 41) to another system or the recirculation of the emulsion or dispersion (41).
14) Dispositif selon l'une quelconque des revendications 10 à 13, caractérisé en ce que le système de mise en vibration (51) du coφs poreux (24) est constitué d'un bobinage (27) relié à une source de courant alternatif (4) entourant l'enveloppe (23) perméable aux ondes magnétiques générées par le bobinage (27), le coφs poreux (24) étant réalisé en matériau magnétostrictif.14) Device according to any one of claims 10 to 13, characterized in that the vibrating system (51) of the porous coφs (24) consists of a coil (27) connected to an AC source ( 4) surrounding the envelope (23) permeable to the magnetic waves generated by the coil (27), the porous coφs (24) being made of magnetostrictive material.
15) Dispositif selon l'une quelconque des revendications 10 à 13, caractérisé en ce que le système de mise en vibration (151) du coφs poreux (24) est constitué d'une tige conductrice (28) disposée coaxialement au coφs poreux (24), d'une enveloppe (23) conductrice, ladite tige conductrice (28) et ladite enveloppe (23) étant reliées à une source de courant alternatif (4), le coφs poreux (24) étant constitué d'un matériau piézoélectrique. 16) Dispositif selon la revendication 15, caractérisé en ce que la tige conductrice (28) et/ou la surface du coφs poreux (24) sont recouvertes d'un isolant (45 ;47).15) Device according to any one of claims 10 to 13, characterized in that the vibrating system (151) of the porous coφs (24) consists of a conductive rod (28) arranged coaxially with the porous coφs (24), a conductive envelope (23), said conductive rod (28) and said envelope (23) being connected to an alternating current source (4), the porous coφs (24) consisting of a piezoelectric material. 16) Device according to claim 15, characterized in that the conductive rod (28) and / or the surface of the porous coφs (24) are covered with an insulator (45; 47).
17) Dispositif selon l'une quelconque des revendications 10 à 13, caractérisé en ce que le système de mise en vibration (251) du coφs poreux (24) est constitué de deux transducteurs (29, 29') fixés aux extrémités (43) du coφs poreux (24) et reliés à une source de courant alternatif (4), lesdits transducteurs (29, 29') étant constitués d'un matériau piézoélectrique.17) Device according to any one of claims 10 to 13, characterized in that the vibrating system (251) of the porous coφs (24) consists of two transducers (29, 29 ') attached to the ends (43) porous coφs (24) and connected to a source of alternating current (4), said transducers (29, 29 ') being made of a piezoelectric material.
18) Dispositif selon la revendication 17, caractérisé en ce que chaque transducteur (290, 290') comporte un moyen de support (291) fixé à l'enveloppe (23), ledit moyen de support (291) comportant un évidement (52) dans lequel est positionnée une extrémité (43) du coφs poreux (24), ledit moyen de support (291) comportant au moins une paire de trous radiaux (293a, 293b), chaque paire contenant un élément piézoélectrique (294) dans un trou et un moyen élastique de sollicitation (295) dans l'autre trou de la même paire (293a, 293b) pour maintenir l'élément piézoélectrique (294) en appui contre le coφs poreux (24), les trous d'une même paire (293a, 293b) étant diamétralement opposés.18) Device according to claim 17, characterized in that each transducer (290, 290 ') comprises a support means (291) fixed to the casing (23), said support means (291) having a recess (52) in which is positioned an end (43) of the porous coφs (24), said support means (291) having at least one pair of radial holes (293a, 293b), each pair containing a piezoelectric element (294) in a hole and an elastic biasing means (295) in the other hole of the same pair (293a, 293b) for holding the piezoelectric element (294) against the porous coφs (24), the holes of the same pair (293a) , 293b) being diametrically opposed.
19) Dispositif selon la revendication 18, caractérisé en ce que le moyen de support (291) comporte deux paires de trous (293a, 293b), les deux paires de trous (293a, 293b) étant disposés dans des directions peφendiculaires, et en ce que les deux éléments piézoélectriques (294) sont alimentés par des signaux décalés d'un quart de période l'un par rapport à l'autre, et en association avec les ressorts de précontrainte (295), engendrent un déplacement du coφs poreux (24) selon une trajectoire globalement circulaire. 19) Device according to claim 18, characterized in that the support means (291) comprises two pairs of holes (293a, 293b), the two pairs of holes (293a, 293b) being arranged in peφendicular directions, and in that that the two piezoelectric elements (294) are powered by signals shifted by a quarter of a period relative to each other, and in association with the prestressing springs (295), cause a displacement of the porous coφs (244). ) in a globally circular path.
EP03778394A 2002-10-15 2003-10-15 Method and device for making a dispersion or an emulsion Expired - Lifetime EP1551540B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0212803A FR2845619B1 (en) 2002-10-15 2002-10-15 DEVICE AND METHOD FOR MANUFACTURING MIXTURE, DISPERSION OR EMULSION OF AT LEAST TWO NON-MISCIBLE REPUTABLE FLUIDS
FR0212803 2002-10-15
PCT/FR2003/003035 WO2004035190A1 (en) 2002-10-15 2003-10-15 Method and device for making a dispersion or an emulsion

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EP1551540B1 EP1551540B1 (en) 2006-04-26

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EP (1) EP1551540B1 (en)
CN (1) CN1711129B (en)
AT (1) ATE324174T1 (en)
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BR (1) BR0315292B1 (en)
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US7622510B2 (en) 2009-11-24
AU2003285402B2 (en) 2008-12-04
CA2501727C (en) 2011-05-24
AU2003285402A1 (en) 2004-05-04
US20060164912A1 (en) 2006-07-27
EP1551540B1 (en) 2006-04-26
FR2845619A1 (en) 2004-04-16
DE60304883T2 (en) 2007-05-03
CN1711129B (en) 2010-05-26
ES2264016T3 (en) 2006-12-16
WO2004035190A1 (en) 2004-04-29
BR0315292A (en) 2005-08-30
ATE324174T1 (en) 2006-05-15
BR0315292B1 (en) 2011-07-12
DE60304883D1 (en) 2006-06-01
CN1711129A (en) 2005-12-21
FR2845619B1 (en) 2005-01-21
CA2501727A1 (en) 2004-04-29

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