EP1467810A1 - Shaking device and method, particularly for dispersing or emulsifying two immiscible fluids - Google Patents

Shaking device and method, particularly for dispersing or emulsifying two immiscible fluids

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Publication number
EP1467810A1
EP1467810A1 EP03712232A EP03712232A EP1467810A1 EP 1467810 A1 EP1467810 A1 EP 1467810A1 EP 03712232 A EP03712232 A EP 03712232A EP 03712232 A EP03712232 A EP 03712232A EP 1467810 A1 EP1467810 A1 EP 1467810A1
Authority
EP
European Patent Office
Prior art keywords
hollow axis
lining
liquids
axis
mixing element
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.)
Withdrawn
Application number
EP03712232A
Other languages
German (de)
French (fr)
Inventor
Daniel Cuzin
Marc Baroni
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.)
Arkema France SA
Original Assignee
Atofina SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Atofina SA filed Critical Atofina SA
Publication of EP1467810A1 publication Critical patent/EP1467810A1/en
Withdrawn legal-status Critical Current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
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/43—Mixing liquids with liquids; Emulsifying using driven stirrers
    • B01F23/431—Mixing liquids with liquids; Emulsifying using driven stirrers the liquids being introduced from the outside through or along the axis of a rotating stirrer, e.g. the stirrer rotating due to the reaction of the introduced liquid
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/11—Stirrers characterised by the configuration of the stirrers
    • B01F27/115—Stirrers characterised by the configuration of the stirrers comprising discs or disc-like elements essentially perpendicular to the stirrer shaft axis
    • B01F27/1152—Stirrers characterised by the configuration of the stirrers comprising discs or disc-like elements essentially perpendicular to the stirrer shaft axis with separate elements other than discs fixed on the discs, e.g. vanes fixed on the discs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/11—Stirrers characterised by the configuration of the stirrers
    • B01F27/118—Stirrers in the form of brushes, sieves, grids, chains or springs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/81—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis the stirrers having central axial inflow and substantially radial outflow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/21—Mixers with rotary stirring devices in fixed receptacles; Kneaders characterised by their rotating shafts
    • B01F27/2122—Hollow shafts

Definitions

  • the invention relates to a stirring device and method, in particular applied to the dispersion or the emulsion of two immiscible liquids.
  • rotary agitators comprising one or more mobiles fixed on a shaft.
  • the shear, the turbulence and the circulation that the agitator introduces into the liquid to be mixed then depend in particular on the characteristics of the mobile, in particular on its geometry.
  • agitators examples include the rotor and stator mixers. Devices of this kind are marketed by Rayneri under the brand name Ultramix and by
  • the static mixer requires the circulation of the liquid to be mixed. Thus, most often, it will be necessary to resort to a pump. These devices are by otherwise not very suitable for the preparation of dispersions or emulsions of immiscible liquids.
  • English Patent No. 237,325 describes a device for mixing, emulsifying or atomizing immiscible liquids or gas-liquid mixtures.
  • This device consists of two coaxial discs mounted on an axis, separated by an annular space occupied by a lining permeable to fluids.
  • the fluid to be treated is brought by a tube to the center of the assembly constituted by the discs and the lining.
  • the centrifugal force expels the fluid through the packing, which plays the same role as a static mixer by dividing the flow of liquid and imposing shear forces on it, which leads to a mixture more and more intimate when the fluid progresses from the center of the assembly to its periphery.
  • U.S. Patent No. 6,280,078 describes a liquid mixing and aeration device composed of a concentric stack of rings of the same outside diameter and decreasing inside diameter fixed on a common axis and separated from each other by wedges delimiting between the rings free spaces allowing the passage of the liquid.
  • the device is immersed in the liquid to be mixed or aerated. When it is rotated, the centrifugal force causes the liquid, and, if necessary, air to be drawn above the free surface of the liquid, and expelled through the free spaces which separate the rings.
  • the apparatus described in this US Pat. No. 6,280,078, which is especially suitable for aeration of liquids, does not include any particular device intended to cause intimate mixing of the liquids to be mixed, in the case of the mixture of two immiscible liquids .
  • the present invention aims to provide a device and a stirring method, in particular for the dispersion and emulsification of immiscible liquids, which does not have the drawbacks of the prior art.
  • the subject of the invention is therefore a rotary stirring device comprising a mixing element operating according to the principle of the static mixer, fixed radially on a hollow axis, this mixing element comprising a cavity occupied by a lining and communicating with the space inside the hollow axis and the fluid medium to be agitated.
  • the mixing element comprises: two discs drilled in their center; - a fixing device making the two discs integral with each other by delimiting a space between them; and a lining arranged in the space thus delimited, the hollow axis being formed of an upper part secured to one of the discs and of a lower part secured to the other disc.
  • one or more openings in the upper and lower part of the hollow axis allow the fluids to be mixed to circulate in the axis and in the packing.
  • the fixing between the first and the second disc is carried out by one or more spacers.
  • the opening in the lower part of the hollow axis is formed by its end.
  • the opening in the upper part of the hollow axis consists of an opening formed on the side of the hollow axis.
  • one or more pipes are fixed radially on the hollow axis. They communicate with the interior space of the axis and are filled with packing similar to the types of packing used in static mixers of the prior art.
  • the lining advantageously consists of a set of solid elements of suitable material, that is to say in particular of material inert with respect to the fluids to be mixed.
  • the solid elements can be for example of metallic material, plastic, ceramic or glass. They can be arranged in a regular arrangement or not inside the cavity constituting the free space of the mixing element.
  • the lining will advantageously be fixed in the cavity so as to prevent its displacement or its loss under the movement of the fluids to be mixed.
  • the filling may in particular be composed of one or more layers of mesh.
  • This mesh is advantageously metallic.
  • It can for example comprise two "layers" separated by a space forming a mixing zone, possibly provided with a perforated plate possibly wavy at its periphery or with a mesh having a larger mesh opening.
  • Another object of the invention is a process for preparing a dispersion or emulsion of immiscible liquids by means of a rotary stirring device comprising a mixing element operating according to the principle of the static mixer, fixed radially on an axis hollow, this mixing element comprising a cavity occupied by a lining, said cavity communicating on the one hand with the interior space of the hollow axis, on the other hand with the fluid medium to be agitated, in which the agitator is placed in rotation, the liquids to be mixed are sucked through hollow axes under the effect of centrifugal force, mix intimately by crossing the packing before being expelled at the periphery of the packing.
  • Another object of the invention is the use of the device according to the invention for the preparation of dispersions and / or emulsions of immiscible liquids.
  • the device according to the embodiment illustrated in the single figure comprises the following elements: a first upper part comprising a first disc 5 fixed by any known mechanical means (for example welding, screwing) to the lower end of a hollow axis 1
  • the hollow axis 1 is pierced near its upper end with a lateral orifice 6 allowing the circulation of the liquid in which the device is immersed;
  • the lower end of the hollow axis 2 is open and allows free passage to the liquid in which the device is immersed.
  • the two discs 5, 5 ' are made integral with one another, while providing a space between them by any suitable means.
  • this means consists of several spacers located on the periphery of the discs and regularly distributed, for example at 120 ° from one another, and providing between the discs a cylindrical space.
  • the number of spacers connecting the two discs will preferably be proportional to the size of the device. If only one spacer is used, balance will be required to ensure proper rotation of the assembly.
  • the space between the discs 5, 5 ' is filled with a lining forming baffles.
  • Such a lining is preferably composed of a stack of several layers of metal grids cut into the shape of a disc of the same diameter as the discs 5, 5 '.
  • a solid axis making it possible to couple the device, either directly or via of a speed reducer, to a motor capable of imparting to it a rotational movement.
  • the hollow axis 1 and the disc 5 on the one hand, the hollow axis 2 and the disc 5 'on the other hand each form an assembly, the axis and the disc being made integral one of the 'other by any suitable means (welding, screwing, etc.).
  • the discs 5, 5 ′ can in principle be replaced by other elements considered to be equivalent when they define a mixing space comprising the linings, connected to the two hollow axes and allowing a radial extraction of the resulting mixture.
  • These elements are such that they allow good rotation of the assembly.
  • the liquids to be mixed are introduced into a suitable tank in which the agitator is placed.
  • the interface between the two liquids is located at the level of the lining, that is to say that each axis is immersed in a separate liquid.
  • the device according to the invention allows the preparation of an emulsion of two liquids at a much lower speed than the known stator rotor agitators.
  • a stirring device according to the embodiment indicated in the figure was used to disperse a mixture of water and standard multigrade engine oil.
  • a stable emulsion was obtained in less than 5 minutes with a rotation speed of only 60 rpm for a disc diameter of 11 cm.
  • the method according to the invention consists in using the device according to the invention to produce a dispersion or emulsion of immiscible liquids. This process can be continuous or discontinuous.
  • the method and the device according to the invention therefore make it possible to produce a mixture in a simple, flexible, rapid and inexpensive manner, effective at low speed of rotation, and particularly suitable for the dispersion or emulsification of immiscible liquids.
  • the invention makes it possible to mix poorly compatible liquid constituents before reaction or polymerization. Since there is no vortex, the invention makes it possible to work with reduced amounts of surfactants and to avoid foaming.
  • the agitator according to the invention promotes liquid / liquid transfers by increasing the specific surface, promotes the rapid dispersion of liquids or solids in a liquid without shearing, therefore without heating.
  • a Rushton turbine, a rotor and stator mixer from the aforementioned company IKA and a device according to the invention were compared with each other.
  • the transparent test tank had a diameter of 28 cm, was equipped with four counter-blades on its periphery arranged symmetrically and contained about 20 liters of liquids.
  • the Rushton turbine (diameter 10cm) and the device according to the invention (diameter 11cm) were introduced (in three parallel tests) into the test tank containing 50% "of oil and 50% of water (% by volume) and driven in rotation by means of a variable speed stirring motor.
  • the interface between oil and water disappears very quickly, the viscosity changes rapidly and stabilizes at 560 cps at 300 rpm and at 620 cps at 500 rpm .
  • the solution is of a milky white color and it is still possible to distinguish with the naked eye a few drops of oil whose size is of the order of 0.5 mm and which have not been dispersed. No vortex occurs and the surface of the agitated medium remains flat.
  • the device according to the invention allows pumping and quickly ensures great homogeneity of the treated solution, without causing a vortex. Unlike the IKA mixer, the device according to the invention does not need a loop. It is therefore much more flexible than the IKA mixer.
  • Example 1 the time required for decanting the emulsified mixtures in Example 1 was compared with a device according to the invention, that is to say the time necessary for the two phases to return to their initial state. This time depends on the stirring speed:

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Mixers With Rotating Receptacles And Mixers With Vibration Mechanisms (AREA)

Abstract

The invention relates to a rotating shaking device comprising a mixing element operating according to the principle of a static mixer. The inventive mixing element is radially fixed on a hollow axle (1, 2) and has a cavity filled by a lining. Said cavity communicates with the interior space of the hollow axle and the fluid medium to be shaken. The invention also relates to a shaking method for which said device is used.

Description

DISPOSITIF ET PROCEDE D'AGITATION EN PARTICULIER DEVICE AND METHOD FOR SHAKING IN PARTICULAR
POUR LA DISPERSION OU L'EMULSIFICATIONFOR DISPERSION OR EMULSIFICATION
DE DEUX LIQUIDES NON MISCIBLESTWO NON-MISCIBLE LIQUIDS
L'invention concerne un dispositif et un procédé d'agitation, en particulier appliqué à la dispersion ou l'émulsion de deux liquides non miscibles.The invention relates to a stirring device and method, in particular applied to the dispersion or the emulsion of two immiscible liquids.
On connaît les agitateurs rotatifs comprenant un ou plusieurs mobiles fixés sur un arbre. Le cisaillement, la turbulence et la circulation que l'agitateur introduit dans le liquide à mélanger dépendent alors notamment des caractéristiques du mobile, en particulier de sa géométrie.There are known rotary agitators comprising one or more mobiles fixed on a shaft. The shear, the turbulence and the circulation that the agitator introduces into the liquid to be mixed then depend in particular on the characteristics of the mobile, in particular on its geometry.
Pour la dispersion ou l'émulsification de liquides non miscibles, il est important que l'agitateur impartisse un fort cisaillement.For the dispersion or emulsification of immiscible liquids, it is important that the agitator impart a strong shear.
Des exemples de tels agitateurs sont les mélangeurs à rotor et stator. Des dispo- si tifs de ce genre sont commercialisés par Rayneri sous la marque Ultramix et parExamples of such agitators are the rotor and stator mixers. Devices of this kind are marketed by Rayneri under the brand name Ultramix and by
IKA sous la marque Ultra Turrax. Le rotor, par exemple une turbine, est monté à l'intérieur d'une pièce fixe, le stator. Le déplacement relatif du rotor par rapport au stator engendre alors des forces de cisaillement qui provoquent la dispersion ou l'émulsification des liquides. On connaît aussi par le document "Development of self-inducing disperser for gas/liquid and liquid/liquid Systems", Second European Conférence on Mixing, 30th IKA under the Ultra Turrax brand. The rotor, for example a turbine, is mounted inside a fixed part, the stator. The relative displacement of the rotor relative to the stator then generates shear forces which cause the dispersion or the emulsification of the liquids. We also know from the document "Development of self-inducing disperser for gas / liquid and liquid / liquid Systems", Second European Conference on Mixing, 30 th
March-lst April 1977, une technique de mélange basée sur le cisaillement induit par la force centrifuge à laquelle est soumis le fluide, lié à l'effet Venturi résultant du dessin particulier du mobile d'agitation . Par ailleurs, on connaît également des mélangeurs statiques dans lesquels le flux de liquide traverse successivement une série d'éléments de mélange fixes qui dévient et divisent le flux. L'efficacité de l'appareil est liée à la géométrie des éléments de mélange et à leur nombre.March-l st April 1977, a mixing technique based on the shear induced by the centrifugal force to which the fluid is subjected, linked to the Venturi effect resulting from the particular design of the stirring mobile. Furthermore, static mixers are also known in which the liquid flow passes successively through a series of fixed mixing elements which deflect and divide the flow. The efficiency of the device is linked to the geometry of the mixing elements and their number.
Cependant, les deux types de dispositifs présentent des inconvénients. En effet, pour répondre à la nécessité de créer un cisaillement élevé au sein du liquide, les agitateurs à rotor et stator sont des dispositifs mécaniques complexes en raison de la faible dimension de l'entrefer qui implique de sévères contraintes sur les tolérances d'usinage et d'alignement, de la géométrie des petites perforations du stator et de la vitesse élevée du rotor. Par ailleurs, la dissipation importante d'énergie dans un petit volume conduit à un échauffement pouvant avoir une influence sur les fluides à mélanger, voire entraîner des problèmes de sécurité.However, both types of devices have drawbacks. Indeed, to meet the need to create a high shear within the liquid, the rotor and stator agitators are complex mechanical devices because of the small size of the air gap which implies severe constraints on the machining tolerances and alignment, the geometry of the small perforations in the stator and the high speed of the rotor. Furthermore, the significant dissipation of energy in a small volume leads to overheating which can have an influence on the fluids to be mixed, or even lead to safety problems.
Le mélangeur statique nécessite la mise en circulation du liquide à mélanger. Ainsi, le plus souvent, il faudra recourir à une pompe. Ces dispositifs sont par ailleurs peu adaptés pour la préparation de dispersions ou d'émulsions de liquides non miscibles.The static mixer requires the circulation of the liquid to be mixed. Thus, most often, it will be necessary to resort to a pump. These devices are by otherwise not very suitable for the preparation of dispersions or emulsions of immiscible liquids.
Le brevet anglais n° 237 325 décrit un dispositif pour le mélange, l'émulsification ou l'atomisation de liquides immiscibles ou de mélanges gaz- liquide. Ce dispositif est constitué de deux disques coaxiaux montés sur un axe, séparés par un espace annulaire occupé par un garnissage perméable aux fluides. Le fluide à traiter est amené par une tubulure au centre de l'assemblage constitué par les disques et le garnissage. Quand le dispositif est mis en rotation, la force centrifuge expulse le fluide à travers le garnissage, qui joue le même rôle qu'un mélangeur statique en divisant le flux de liquide et en lui imposant des forces de cisaillement, ce qui conduit à un mélange de plus en plus intime quand le fluide progresse du centre de l'assemblage vers sa périphérie.English Patent No. 237,325 describes a device for mixing, emulsifying or atomizing immiscible liquids or gas-liquid mixtures. This device consists of two coaxial discs mounted on an axis, separated by an annular space occupied by a lining permeable to fluids. The fluid to be treated is brought by a tube to the center of the assembly constituted by the discs and the lining. When the device is rotated, the centrifugal force expels the fluid through the packing, which plays the same role as a static mixer by dividing the flow of liquid and imposing shear forces on it, which leads to a mixture more and more intimate when the fluid progresses from the center of the assembly to its periphery.
Le brevet américain n° 2 814 527 décrit un atomiseur centrifuge dont le principe de base du fonctionnement est semblable à celui du dispositif décrit dans le brevet anglais précité, le liquide étant atomisé en circulant sous l'effet de la force centrifuge au travers d'un ensemble de chicanes disposées selon une géométrie particulière sur le pourtour de l'atomiseur.US Patent No. 2,814,527 describes a centrifugal atomizer whose basic operating principle is similar to that of the device described in the aforementioned English patent, the liquid being atomized by circulating under the effect of centrifugal force through a set of baffles arranged in a particular geometry around the periphery of the atomizer.
Les appareils décrits dans ces brevets anglais et américain sont bien adaptés à l'atomisation de liquides ou au mélange de liquides dans des procédés de type continu, mais ils ne conviennent pas pour réaliser le mélange ou l'émulsification de deux liquides immiscibles dans un procédé de type batch (discontinu) où le mobile d'agitation est immergé dans les liquides à mélanger pendant toute l'opération.The devices described in these English and American patents are well suited for atomizing liquids or for mixing liquids in continuous type processes, but they are not suitable for mixing or emulsifying two immiscible liquids in a process. batch type (discontinuous) where the agitator is immersed in the liquids to be mixed during the whole operation.
Le brevet américain n° 6 280 078 décrit un appareil de mélange et d'aération de liquide composé d'un empilement concentrique d'anneaux de même diamètre extérieur et de diamètre intérieur décroissant fixés sur un axe commun et séparés les uns des autres par des cales délimitant entre les anneaux des espaces libres permettant le passage du liquide. Le dispositif est plongé dans le liquide à mélanger ou à aérer. Quand il est mis en rotation, la force centrifuge provoque l'aspiration du liquide, et, le cas échéant, de l'air au-dessus de la surface libre du liquide, et leur expulsion au travers des espaces libres qui séparent les anneaux.U.S. Patent No. 6,280,078 describes a liquid mixing and aeration device composed of a concentric stack of rings of the same outside diameter and decreasing inside diameter fixed on a common axis and separated from each other by wedges delimiting between the rings free spaces allowing the passage of the liquid. The device is immersed in the liquid to be mixed or aerated. When it is rotated, the centrifugal force causes the liquid, and, if necessary, air to be drawn above the free surface of the liquid, and expelled through the free spaces which separate the rings.
L'appareil décrit dans ce brevet américain n° 6 280 078, qui est surtout adapté à l'aération des liquides, ne comprend aucun dispositif particulier destiné à provoquer un mélange intime des liquides à mélanger, dans le cas du mélange de deux liquides immiscibles. La présente invention a pour but de proposer un dispositif et un procédé d'agitation, en particulier pour la dispersion et l'émulsification de liquides non miscibles, qui ne présente pas les inconvénients de l'art antérieur. L'invention a donc comme objet un dispositif rotatif d'agitation comprenant un élément de mélange fonctionnant selon le principe du mélangeur statique, fixé radialement sur un axe creux, cet élément de mélange comportant une cavité occupée par un garnissage et communiquant avec l'espace intérieur de l'axe creux et le milieu fluide à agiter.The apparatus described in this US Pat. No. 6,280,078, which is especially suitable for aeration of liquids, does not include any particular device intended to cause intimate mixing of the liquids to be mixed, in the case of the mixture of two immiscible liquids . The present invention aims to provide a device and a stirring method, in particular for the dispersion and emulsification of immiscible liquids, which does not have the drawbacks of the prior art. The subject of the invention is therefore a rotary stirring device comprising a mixing element operating according to the principle of the static mixer, fixed radially on a hollow axis, this mixing element comprising a cavity occupied by a lining and communicating with the space inside the hollow axis and the fluid medium to be agitated.
Selon une réalisation particulière de l'invention, l'élément de mélange comprend : deux disques percés en leur centre ; - un dispositif de fixation rendant les deux disques solidaires l'un de l'autre en délimitant un espace entre eux ; et un garnissage disposé dans l'espace ainsi délimité, l'axe creux étant formé d'une partie supérieure solidaire d'un des disques et d'une partie inférieure solidaire de l'autre disque.According to a particular embodiment of the invention, the mixing element comprises: two discs drilled in their center; - a fixing device making the two discs integral with each other by delimiting a space between them; and a lining arranged in the space thus delimited, the hollow axis being formed of an upper part secured to one of the discs and of a lower part secured to the other disc.
En particulier, une ou plusieurs ouvertures ménagées dans la partie supérieure et inférieure de l'axe creux permettent aux fluides à mélanger de circuler dans l'axe et dans le garnissage.In particular, one or more openings in the upper and lower part of the hollow axis allow the fluids to be mixed to circulate in the axis and in the packing.
Selon un mode de réalisation, la fixation entre le premier et le deuxième disque est réalisée par une ou plusieurs entretoises.According to one embodiment, the fixing between the first and the second disc is carried out by one or more spacers.
De préférence, l'ouverture dans la partie inférieure de l'axe creux est constituée par son extrémité.Preferably, the opening in the lower part of the hollow axis is formed by its end.
Avantageusement, l'ouverture dans la partie supérieure de l'axe creux est constituée d'une ouverture ménagée au flanc de l'axe creux.Advantageously, the opening in the upper part of the hollow axis consists of an opening formed on the side of the hollow axis.
Selon un autre mode de réalisation, une ou plusieurs tubulures sont fixées radialement sur l'axe creux. Elles communiquent avec l'espace intérieur de l'axe et sont remplies de garnissage analogue aux types de garnissages utilisés dans les mélangeurs statiques de l'art antérieur.According to another embodiment, one or more pipes are fixed radially on the hollow axis. They communicate with the interior space of the axis and are filled with packing similar to the types of packing used in static mixers of the prior art.
Le garnissage est avantageusement constitué d'un ensemble d'éléments solides en matériau adapté, c'est-à-dire notamment en matériau inerte vis-à-vis des fluides à mélanger. Les éléments solides peuvent être par exemple en matériau métallique, plastique, céramique ou en verre. Ils peuvent être disposés selon un arrangement régulier ou non à l'intérieur de la cavité constituant l'espace libre de l'élément de mélange. Le garnissage sera avantageusement fixe dans la cavité de manière à prévenir son déplacement ou sa perte sous le mouvement des fluides à mélanger.The lining advantageously consists of a set of solid elements of suitable material, that is to say in particular of material inert with respect to the fluids to be mixed. The solid elements can be for example of metallic material, plastic, ceramic or glass. They can be arranged in a regular arrangement or not inside the cavity constituting the free space of the mixing element. The lining will advantageously be fixed in the cavity so as to prevent its displacement or its loss under the movement of the fluids to be mixed.
Le garnissage peut être en particulier composé d'une ou plusieurs couches de grillage. Ce grillage est avantageusement métallique.The filling may in particular be composed of one or more layers of mesh. This mesh is advantageously metallic.
Il peut par exemple comprendre deux "couches" séparées par un espace formant une zone de mélange , éventuellement muni d'une plaque perforée éventuellement ondulée à sa périphérie ou d'un grillage ayant une ouverture de maille plus grande.It can for example comprise two "layers" separated by a space forming a mixing zone, possibly provided with a perforated plate possibly wavy at its periphery or with a mesh having a larger mesh opening.
Un autre objet de l'invention est un procédé de préparation d'une dispersion ou émulsion de liquides non miscibles au moyen d'un dispositif d'agitation rotatif comprenant un élément de mélange fonctionnant selon le principe du mélangeur statique, fixé radialement sur un axe creux, cet élément de mélange comportant une cavité occupée par un garnissage, ladite cavité communiquant d'une part avec l'espace intérieur de l'axe creux, d'autre part avec le milieu fluide à agiter, dans lequel l'agitateur est mis en rotation, les liquides à mélanger sont aspirés au travers des axes creux sous l'effet de la force centrifuge, se mélangent intimement en traversant le garnissage avant d'être expulsés à la périphérie du garnissage.Another object of the invention is a process for preparing a dispersion or emulsion of immiscible liquids by means of a rotary stirring device comprising a mixing element operating according to the principle of the static mixer, fixed radially on an axis hollow, this mixing element comprising a cavity occupied by a lining, said cavity communicating on the one hand with the interior space of the hollow axis, on the other hand with the fluid medium to be agitated, in which the agitator is placed in rotation, the liquids to be mixed are sucked through hollow axes under the effect of centrifugal force, mix intimately by crossing the packing before being expelled at the periphery of the packing.
Un autre objet de l'invention est l'utilisation du dispositif selon l'invention pour la préparation de dispersions et/ou d'émulsions de liquides non miscibles.Another object of the invention is the use of the device according to the invention for the preparation of dispersions and / or emulsions of immiscible liquids.
Le dispositif selon l'invention est expliqué plus en détail en référence à la figure unique en annexe qui montre un mode de réalisation d'un agitateur selon l'invention.The device according to the invention is explained in more detail with reference to the single figure in the appendix which shows an embodiment of an agitator according to the invention.
Le dispositif selon le mode de réalisation illustré à la figure unique comprend les éléments suivants : une première partie supérieure comprenant un premier disque 5 fixé par tout moyen mécanique connu (par exemple soudage, vissage) à l'extrémité inférieure d'un axe creux 1. L'axe creux 1 est percé près de son extrémité supérieure d'un orifice latéral 6 permettant la circulation du liquide dans lequel est plongé le dispositif ; une partie inférieure semblable à la partie supérieure, comprenant un deuxième disque 5' fixé par tout moyen mécanique à l'extrémité supérieure d'un axe creux 2. L'extrémité inférieure de l'axe creux 2 est ouverte et laisse libre passage au liquide dans lequel est plongé le dispositif.The device according to the embodiment illustrated in the single figure comprises the following elements: a first upper part comprising a first disc 5 fixed by any known mechanical means (for example welding, screwing) to the lower end of a hollow axis 1 The hollow axis 1 is pierced near its upper end with a lateral orifice 6 allowing the circulation of the liquid in which the device is immersed; a lower part similar to the upper part, comprising a second disc 5 'fixed by any mechanical means to the upper end of a hollow axis 2. The lower end of the hollow axis 2 is open and allows free passage to the liquid in which the device is immersed.
Les deux disques 5, 5' sont rendus solidaires l'un de l'autre, tout en ménageant un espace entre eux par tout moyen convenable. De préférence, ce moyen est constitué de plusieurs entretoises situées sur la périphérie des disques et régulièrement réparties, par exemple à 120° l'une de l'autre, et ménageant entre les disques un espace cylindrique. Le nombre d'entretoises reliant les deux disques sera de préférence proportionnel à la taille du dispositif. En cas d'utilisation d'une seule entretoise, on veillera à l'équilibre pour assurer une bonne rotation de l'ensemble. L'espace ménagé entre les disques 5, 5' est rempli par un garnissage formant des chicanes. Un tel garnissage est de préférence composé d'un empilement de plusieurs couches de grilles métalliques découpées en forme de disque de même diamètre que les disques 5, 5'. A l'extrémité supérieure libre de l'axe creux 1 de la partie supérieure du dispositif est fixée par tout moyen mécanique convenable (par exemple soudage, vissage) un axe plein permettant d'accoupler le dispositif, soit directement, soit par l'intermédiaire d'un réducteur de vitesse, à un moteur susceptible de lui imprimer un mouvement de rotation.The two discs 5, 5 'are made integral with one another, while providing a space between them by any suitable means. Preferably, this means consists of several spacers located on the periphery of the discs and regularly distributed, for example at 120 ° from one another, and providing between the discs a cylindrical space. The number of spacers connecting the two discs will preferably be proportional to the size of the device. If only one spacer is used, balance will be required to ensure proper rotation of the assembly. The space between the discs 5, 5 'is filled with a lining forming baffles. Such a lining is preferably composed of a stack of several layers of metal grids cut into the shape of a disc of the same diameter as the discs 5, 5 '. At the free upper end of the hollow axis 1 of the upper part of the device is fixed by any suitable mechanical means (for example welding, screwing) a solid axis making it possible to couple the device, either directly or via of a speed reducer, to a motor capable of imparting to it a rotational movement.
De préférence, l'axe creux 1 et le disque 5 d'une part, l'axe creux 2 et le disque 5' d'autre part forment chacun un ensemble, l'axe et le disque étant rendus solidaires l'un de l'autre par tout moyen convenable (soudure, vissage etc.).Preferably, the hollow axis 1 and the disc 5 on the one hand, the hollow axis 2 and the disc 5 'on the other hand each form an assembly, the axis and the disc being made integral one of the 'other by any suitable means (welding, screwing, etc.).
Toutefois, les disques 5, 5' peuvent en principe être remplacées par d'autres éléments considérés comme équivalents dès lors qu'ils définissent un espace de mélange comprenant les garnissages, relié aux deux axes creux et permettant une extraction radiale du mélange résultant. Ces éléments sont tels qu'ils autorisent une bonne rotation de l'ensemble. On peut citer à titre d'exemple l'utilisation de plusieurs pales creuses ou de plusieurs tubulures, communiquant avec l'axe et munies chacune individuellement d'éléments d'un garnissage semblable à ceux utilisés dans les mélangeurs statiques.However, the discs 5, 5 ′ can in principle be replaced by other elements considered to be equivalent when they define a mixing space comprising the linings, connected to the two hollow axes and allowing a radial extraction of the resulting mixture. These elements are such that they allow good rotation of the assembly. By way of example, mention may be made of the use of several hollow blades or of several tubes, communicating with the axis and each provided individually with elements of packing similar to those used in static mixers.
On pourrait par ailleurs prévoir des pales (par ex. du type de celles d'un mélangeur Rushton) sur le(s) disque(s) (5,5') afin d'obtenir, au début, un mélange grossier qui est ensuite affiné par l'agitateur selon l'invention. Le fonctionnement de l'agitateur selon l'invention est le suivant :We could also provide blades (eg of the type of those of a Rushton mixer) on the disc (s) (5.5 ') in order to obtain, at the beginning, a coarse mixture which is then refined by the agitator according to the invention. The operation of the agitator according to the invention is as follows:
Les liquides à mélanger sont introduits dans une cuve adaptée dans laquelle est disposé l'agitateur. De préférence, l'interface entre les deux liquides se situe au niveau du garnissage, c'est-à-dire que chaque axe est immergé dans un liquide distinct. Lorsque l'agitateur est mis en rotation, les liquides sont aspirés au travers des axes creux sous l'effet de la force centrifuge et se mélangent intimement en traversant le garnissage formant chicanes avant d'être expulsé à sa périphérie.The liquids to be mixed are introduced into a suitable tank in which the agitator is placed. Preferably, the interface between the two liquids is located at the level of the lining, that is to say that each axis is immersed in a separate liquid. When the agitator is rotated, the liquids are sucked through the hollow axes under the effect of centrifugal force and mix intimately by crossing the lining forming baffles before being expelled at its periphery.
De cette façon, la rotation de l'agitateur permet au garnissage de jouer le rôle d'un mélangeur statique, renforçant ainsi l'effet de mélange obtenu.In this way, the rotation of the agitator allows the packing to play the role of a static mixer, thus reinforcing the mixing effect obtained.
En effet, le dispositif selon l'invention permet la préparation d'une émulsion de deux liquides à vitesse bien plus faible que les agitateurs rotor stator connus.Indeed, the device according to the invention allows the preparation of an emulsion of two liquids at a much lower speed than the known stator rotor agitators.
Ainsi, un dispositif d'agitation selon le mode de réalisation indiqué à la figure a été utilisé pour disperser un mélange d'eau et d'huile moteur multigrade standard. Une émulsion stable a été obtenue en moins de 5 minutes avec une vitesse de rotation de 60 t/min seulement pour un diamètre des disques de 11 cm. Le procédé selon l'invention consiste à utiliser le dispositif selon l'invention pour réaliser une dispersion ou émulsion de liquides non miscibles. Ce procédé peut être continu ou discontinu. Le procédé et le dispositif selon l'invention permettent donc de réaliser un mélange de manière simple, souple, rapide et peu onéreuse, efficace à faible vitesse de rotation, et particulièrement adaptée pour la dispersion ou l'émulsification de liquides non miscibles. Ainsi, l'invention permet de mélanger des constituants liquides peu compatibles avant réaction ou polymérisation. Etant donné qu'il ne se produit pas de vortex, l'invention permet de travailler avec des quantités de tensio-actifs réduites et d'éviter la formation de mousse.Thus, a stirring device according to the embodiment indicated in the figure was used to disperse a mixture of water and standard multigrade engine oil. A stable emulsion was obtained in less than 5 minutes with a rotation speed of only 60 rpm for a disc diameter of 11 cm. The method according to the invention consists in using the device according to the invention to produce a dispersion or emulsion of immiscible liquids. This process can be continuous or discontinuous. The method and the device according to the invention therefore make it possible to produce a mixture in a simple, flexible, rapid and inexpensive manner, effective at low speed of rotation, and particularly suitable for the dispersion or emulsification of immiscible liquids. Thus, the invention makes it possible to mix poorly compatible liquid constituents before reaction or polymerization. Since there is no vortex, the invention makes it possible to work with reduced amounts of surfactants and to avoid foaming.
Comme utilisations particulièrement intéressantes du dispositif et du procédé selon l'invention, on peut citer la préparation de dispersions de liquides incompatibles destinées à des réactions (polymérisation...), de dispersions de latex avec des charges (ces dispersions pouvant alors être réalisées sans utiliser d'anti- mousse), ou d'émulsions destinées à des polymérisations en émulsion.As particularly advantageous uses of the device and of the method according to the invention, mention may be made of the preparation of dispersions of incompatible liquids intended for reactions (polymerization, etc.), dispersions of latex with fillers (these dispersions can then be produced without use antifoam), or emulsions intended for emulsion polymerizations.
L'agitateur selon l'invention favorise les transferts liquide/liquide par augmentation de la surface spécifique, favorise la dispersion rapide de liquides ou de solides dans un liquide sans cisaillement donc sans échauffement.The agitator according to the invention promotes liquid / liquid transfers by increasing the specific surface, promotes the rapid dispersion of liquids or solids in a liquid without shearing, therefore without heating.
ExemplesExamples
Les exemples suivants illustrent la présente invention sans toutefois en limiter la portée.The following examples illustrate the present invention without, however, limiting its scope.
Exemple 1Example 1
Dans cet exemple, on a comparé entre eux une turbine Rushton, un mélangeur à rotor et stator de la société précitée IKA et un dispositif selon l'invention. La cuve d'essai transparente avait un diamètre de 28 cm, était équipée de quatre contrepales sur sa périphérie disposées de façon symétrique et contenait environ 20 litres de liquides.In this example, a Rushton turbine, a rotor and stator mixer from the aforementioned company IKA and a device according to the invention were compared with each other. The transparent test tank had a diameter of 28 cm, was equipped with four counter-blades on its periphery arranged symmetrically and contained about 20 liters of liquids.
La turbine Rushton (diamètre 10cm) et le dispositif selon l'invention (diamètre 11cm) ont été introduits (dans trois essais parallèles) dans la cuve d'essai contenant 50%» d'huile et 50% d'eau (% volumiques) et entraînés en rotation au moyen d'un moteur d'agitation à vitesse variable.The Rushton turbine (diameter 10cm) and the device according to the invention (diameter 11cm) were introduced (in three parallel tests) into the test tank containing 50% "of oil and 50% of water (% by volume) and driven in rotation by means of a variable speed stirring motor.
L'évolution de la viscosité du contenu de la cuve est suivie au moyen d'un viscosimètre Brookfields (module 2, vitesse 20).The evolution of the viscosity of the contents of the tank is monitored using a Brookfields viscometer (module 2, speed 20).
Avec la Turbine Rushton (6 pales) tournant à 300 tr/min et 500 tr/min, l'interface entre l'huile et l'eau disparaît instantanément mais la solution est instable et l'échantillon prélevé décante partiellement avant que la mesure de viscosité soit faite. La viscosité n'est pas mesurable au Brookfields avec le module 2 (vitesse 20).With the Rushton Turbine (6 blades) rotating at 300 rpm and 500 rpm, the interface between oil and water disappears instantly but the solution is unstable and the sample taken partially settles before the measurement of viscosity be made. The viscosity cannot be measured at Brookfields with module 2 (speed 20).
Il y a formation d'un vortex. Avec le mélangeur IKA, de type rotor-stator et pompe (vitesse de rotation du rotor 3000tr/min, débit 1 1/s) placé en boucle de dérivation sur un réacteur contenant 30 litres de mélange « eau-huile », on essaie d'émulsionner directement le mélange « eau-huile », mais l'émulsion ne se stabilise pas et il n'est pas possible d'obtenir directement un produit homogène et un prélèvement représentatif de l'ensemble de la solution. Le système rotor-stator n'a pas le pouvoir de mélanger les liquides et ne parvient pas à faire un produit homogène au bout de 6 passages. Un prémélange (avec le dispositif selon l'invention) est nécessaire pour que le mélangeur IKA. fournisse une émulsion (d'une qualité sensiblement identique à celle obtenue avec le dispositif selon l'invention).There is a vortex. With the IKA mixer, rotor-stator type and pump (rotor rotation speed 3000 rpm, flow rate 1 1 / s) placed in bypass loop on a reactor containing 30 liters of “water-oil” mixture, we try to '' directly emulsify the “water-oil” mixture, but the emulsion does not stabilize and it is not possible to directly obtain a homogeneous product and a sample representative of the entire solution. The rotor-stator system does not have the power to mix liquids and does not manage to make a homogeneous product after 6 passages. A premix (with the device according to the invention) is necessary for the IKA mixer. provide an emulsion (of a quality substantially identical to that obtained with the device according to the invention).
Avec le dispositif selon l'invention, on constate que l'interface entre l'huile et l'eau disparaît très rapidement , la viscosité évolue rapidement et se stabilise à 560 cps à 300 tr/min et à 620 cps à 500 tr/min. La solution est d'une couleur blanc-laiteux et il est encore possible de distinguer à l'œil nu quelques gouttes d'huile dont la taille est de l'ordre de 0,5 mm et qui n'ont pas été dispersées. Il ne se produit pas de vortex et la surface du milieu agité reste plane.With the device according to the invention, it can be seen that the interface between oil and water disappears very quickly, the viscosity changes rapidly and stabilizes at 560 cps at 300 rpm and at 620 cps at 500 rpm . The solution is of a milky white color and it is still possible to distinguish with the naked eye a few drops of oil whose size is of the order of 0.5 mm and which have not been dispersed. No vortex occurs and the surface of the agitated medium remains flat.
Le dispositif selon l'invention permet un pompage et assure rapidement une grande homogénéité de la solution traitée et cela sans provoquer de vortex. Contrairement au mélangeur IKA, le dispositif selon l'invention n'a pas besoin d'une boucle. Il est donc beaucoup plus souple que le mélangeur IKA.The device according to the invention allows pumping and quickly ensures great homogeneity of the treated solution, without causing a vortex. Unlike the IKA mixer, the device according to the invention does not need a loop. It is therefore much more flexible than the IKA mixer.
Exemple 2Example 2
Dans cet exemple, on a comparé le temps nécessaire à la décantation des mélanges émulsionnés à l'exemple 1 avec un dispositif selon l'invention, c'est-à-dire le temps nécessaire pour que les deux phases retrouvent leur état initial. Ce temps dépend de la vitesse d'agitation:In this example, the time required for decanting the emulsified mixtures in Example 1 was compared with a device according to the invention, that is to say the time necessary for the two phases to return to their initial state. This time depends on the stirring speed:
- 2 h 30 pour 300 tr/min- 2 h 30 for 300 rpm
- 5 h pour 500 tr/min- 5 h for 500 rpm
Avec la turbine Rushton, après agitation à 300 tr/min, le retour à l'état initial ne nécessite que 30 minutes, ce qui signifie que l'émulsion était relativement instable. With the Rushton turbine, after stirring at 300 rpm, the return to the initial state requires only 30 minutes, which means that the emulsion was relatively unstable.

Claims

REVENDICATIONS
1.- Dispositif d'agitation rotatif comprenant un élément de mélange fonctionnant selon le principe du mélangeur statique, fixé radialement sur un axe creux (1,2), cet élément de mélange comportant une cavité occupée par un garnissage, la dite cavité communiquant d'une part avec l'espace intérieur de l'axe creux, d'autre part avec le milieu fluide à agiter.1.- Rotary stirring device comprising a mixing element operating according to the principle of the static mixer, fixed radially on a hollow axis (1,2), this mixing element comprising a cavity occupied by a lining, said cavity communicating d on the one hand with the interior space of the hollow axis, on the other hand with the fluid medium to be agitated.
2.- Dispositif selon la revendication 1, dans lequel l'élément de mélange comprend : deux disques (5,5') percés en leur centre ;2.- Device according to claim 1, wherein the mixing element comprises: two discs (5,5 ') drilled in their center;
- un dispositif de fixation (3) rendant les deux disques (5,5') solidaires l'un de l'autre en délimitant un espace entre eux ; et- a fixing device (3) making the two discs (5.5 ′) integral with one another by delimiting a space between them; and
- un garnissage (4) disposé dans l'espace ainsi délimité, l'axe creux étant formé d'une partie supérieure (1) solidaire du disque (5) et d'une partie inférieure (2) solidaire du disque (5').- a lining (4) disposed in the space thus delimited, the hollow axis being formed of an upper part (1) secured to the disc (5) and a lower portion (2) secured to the disc (5 ') .
3.- Dispositif selon la revendication 2, dans lequel l'axe creux (1,2) comporte une ouverture (6) dans sa partie supérieure et une ouverture (7) dans sa partie infé- rieure .3.- Device according to claim 2, wherein the hollow axis (1,2) has an opening (6) in its upper part and an opening (7) in its lower part.
4.- Dispositif selon l'une des revendications précédentes, dans lequel la fixation entre le premier et le deuxième disque (5,5') est réalisée par une ou plusieurs entretoises.4.- Device according to one of the preceding claims, wherein the fixing between the first and the second disc (5,5 ') is carried out by one or more spacers.
5.- Dispositif selon l'une des revendications précédentes, dans lequel l'ouverture (7) dans l'axe creux (2) est constituée par son extrémité.5.- Device according to one of the preceding claims, wherein the opening (7) in the hollow axis (2) is constituted by its end.
6.- Dispositif selon l'une des revendications précédentes, dans lequel l'ouverture (6) dans l'axe creux (1) est ménagée au flanc de l'axe.6.- Device according to one of the preceding claims, wherein the opening (6) in the hollow axis (1) is formed on the side of the axis.
7.- Dispositif selon l'une des revendications précédentes, dans lequel sont fixées radialement sur l'axe creux (1,2) une ou plusieurs tubulure(s) communiquant avec l'espace intérieur de l'axe et remplies de garnissage.7.- Device according to one of the preceding claims, wherein are fixed radially on the hollow axis (1,2) one or more tubing (s) communicating with the interior space of the axis and filled with packing.
8.- Dispositif selon l'une des revendications précédentes, dans lequel le garnissage (4) est composé d'un ensemble d'éléments solides en matériau métallique, plastique, céramique, verre, disposés selon un arrangement régulier ou non. 8.- Device according to one of the preceding claims, wherein the lining (4) is composed of a set of solid elements of metallic material, plastic, ceramic, glass, arranged in a regular arrangement or not.
9.- Dispositif selon la revendication 8, dans lequel le garnissage (4) est composé d'une ou plusieurs couches de grillage.9.- Device according to claim 8, wherein the lining (4) is composed of one or more layers of mesh.
10.- Dispositif selon la revendication 9, dans lequel le grillage est métallique.10.- Device according to claim 9, wherein the mesh is metallic.
11.- Utilisation du dispositif selon l'une des revendications précédentes pour la préparation de dispersions et/ou d'émulsions de liquides non miscibles.11.- Use of the device according to one of the preceding claims for the preparation of dispersions and / or emulsions of immiscible liquids.
12. Procédé de préparation d'une dispersion ou émulsion de liquides non miscibles au moyen d'un dispositif d'agitation rotatif comprenant un élément de mélange fonctionnant selon le principe du mélangeur statique, fixé radialement sur un axe creux (1,2), cet élément de mélange comportant une cavité occupée par un garnissage (4), ladite cavité communiquant d'une part avec l'espace intérieur de l'axe creux, d'autre part avec le milieu fluide à agiter, dans lequel l'agitateur est mis en rotation, les liquides à mélanger sont aspirés au travers des axes creux sous l'effet de la force centrifuge, se mélangent intimement en traversant le garnissage avant d'être expulsés à la périphérie du garnissage (4).12. Method for preparing a dispersion or emulsion of immiscible liquids by means of a rotary stirring device comprising a mixing element operating according to the principle of the static mixer, fixed radially on a hollow axis (1,2), this mixing element comprising a cavity occupied by a lining (4), said cavity communicating on the one hand with the interior space of the hollow axis, on the other hand with the fluid medium to be agitated, in which the agitator is put in rotation, the liquids to be mixed are sucked through hollow axes under the effect of centrifugal force, mix intimately by crossing the packing before being expelled at the periphery of the packing (4).
13. Procédé selon la revendication 12, dans lequel l'un des liquides entre par la partie supérieure (1) et l'autre par la partie inférieure (2) de l'axe creux.13. The method of claim 12, wherein one of the liquids enters through the upper part (1) and the other through the lower part (2) of the hollow axis.
14. Procédé selon la revendication 12 ou la revendication 13, dans lequel le dispositif d'agitation rotatif est le dispositif selon l'une des revendications 2 à 10.14. The method of claim 12 or claim 13, wherein the rotary stirring device is the device according to one of claims 2 to 10.
15. Procédé selon l'une des revendications 12 à 14, dans lequel l'interface entre les deux liquides se situe au niveau du garnissage (4). 15. Method according to one of claims 12 to 14, wherein the interface between the two liquids is located at the level of the lining (4).
EP03712232A 2002-01-11 2003-01-10 Shaking device and method, particularly for dispersing or emulsifying two immiscible fluids Withdrawn EP1467810A1 (en)

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FR0200306A FR2834652B1 (en) 2002-01-11 2002-01-11 AGITATION DEVICE IN PARTICULAR FOR THE DISPERSION OR EMULSIFICATION OF TWO NON-MISCIBLE LIQUIDS
PCT/FR2003/000073 WO2003057354A1 (en) 2002-01-11 2003-01-10 Shaking device and method, particularly for dispersing or emulsifying two immiscible fluids

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JP2005514195A (en) 2005-05-19
US20050254342A1 (en) 2005-11-17
FR2834652B1 (en) 2004-02-27
WO2003057354A8 (en) 2004-04-29
AU2003216713A1 (en) 2003-07-24
CN1638854A (en) 2005-07-13
WO2003057354A1 (en) 2003-07-17
CA2473098A1 (en) 2003-07-17
FR2834652A1 (en) 2003-07-18

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