EP1262225B1 - Dispositif et procédé de préparation d'emulsions - Google Patents

Dispositif et procédé de préparation d'emulsions Download PDF

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Publication number
EP1262225B1
EP1262225B1 EP02011487A EP02011487A EP1262225B1 EP 1262225 B1 EP1262225 B1 EP 1262225B1 EP 02011487 A EP02011487 A EP 02011487A EP 02011487 A EP02011487 A EP 02011487A EP 1262225 B1 EP1262225 B1 EP 1262225B1
Authority
EP
European Patent Office
Prior art keywords
shaft
housing
membrane
emulsion
membrane units
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.)
Expired - Lifetime
Application number
EP02011487A
Other languages
German (de)
English (en)
Other versions
EP1262225A2 (fr
EP1262225A3 (fr
Inventor
Ursula Dipl.-Ing. Schliessmann
Norbert Dipl.-Ing. Stroh
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.)
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Original Assignee
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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 Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV filed Critical Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Publication of EP1262225A2 publication Critical patent/EP1262225A2/fr
Publication of EP1262225A3 publication Critical patent/EP1262225A3/fr
Application granted granted Critical
Publication of EP1262225B1 publication Critical patent/EP1262225B1/fr
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
    • 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
    • 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
    • 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
    • B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
    • B01F25/3131—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit with additional mixing means other than injector mixers, e.g. screens, baffles or rotating elements
    • 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
    • B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
    • B01F25/3133—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit characterised by the specific design of the injector
    • B01F25/31331—Perforated, multi-opening, with a plurality of holes
    • B01F25/313311—Porous injectors
    • 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
    • B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
    • B01F25/3133—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit characterised by the specific design of the injector
    • B01F25/31333—Rotatable injectors
    • 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
    • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
    • B01F27/271—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed radially between the surfaces of the rotor and the stator
    • 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
    • B01F27/051—Stirrers characterised by their elements, materials or mechanical properties
    • 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
    • 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
    • B01F27/19—Stirrers with two or more mixing elements mounted in sequence on the same axis
    • B01F27/191—Stirrers with two or more mixing elements mounted in sequence on the same axis with similar elements
    • 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 present invention relates to an apparatus and a use of the apparatus for the preparation of emulsions using one or more membranes, through which a dispersed phase of a liquid medium is finely divided into a continuous phase of another liquid medium.
  • the disperse phase is distributed in the form of fine droplets in the continuous phase.
  • the emulsion is selected from an oily and an aqueous phase.
  • rotor-stator systems are simple stirrers, sprocket dispersing machines and colloid mills.
  • the continuous and disperse phases are brought together in a container and mixed together by the operation of the rotor to form an emulsion.
  • the energy consumption for the operation of these devices is very high.
  • a strong evolution of heat often occurs, which can heat the emulsion to undesirably high temperatures.
  • the diameters of the emulsion droplets are between 0.1 and 100 .mu.m, whereby a very broad droplet size distribution is generally present.
  • Another method of making emulsions employs a membrane technique to produce finely divided dispersed phase droplets in the continuous phase.
  • the disperse phase is in this case pressed through the pores of a membrane, so that form drops on the surface of the membrane, which tear off after reaching a critical drop diameter and entrained by the flowing over the surface continuous phase.
  • a tube membrane is used, which is flowed through by a continuous phase.
  • the disperse phase is forced from the outside through the porous system of the tube membrane into the inwardly flowing continuous phase.
  • the flow of the disperse phase is due to an applied transmembrane pressure difference.
  • the actual process of emulsification, ie the formation of drops, takes place on the inner surface of the tube membrane.
  • the drops grow on this surface until the drip-releasing forces become larger than the forces that hold the drop at the respective pore.
  • the droplet is then detached with the diameter reached from the continuous phase, which flows over the membrane surface, and entrained by the flow.
  • the object of the present invention is to provide an apparatus and a process for the preparation of emulsions which are homogeneous Droplet size distribution allows for low energy consumption.
  • the apparatus comprises a housing having an inlet and outlet opening for a continuous phase of a first liquid medium, a shaft rotatably driven in the housing, on or in which a feed channel for a disperse phase of a second liquid medium is formed, and one or more hollow trained membrane body, which are attached to the shaft.
  • the supply channel is connected in the present device via the shaft with the hollow membrane bodies to allow the supply of the disperse phase via the feed channel in the membrane body.
  • the device is characterized in that the membrane body are hollow and a present due to the spaced positions between the membrane bodies intermediate space is filled by an adapted inner contour of the housing while maintaining a small distance to the membrane bodies and the shaft.
  • the continuous phase is introduced into the housing and then or simultaneously the disperse phase via the supply channel to the shaft under pressure in the hollow trained membrane body initiated.
  • the shaft is rotationally driven by a motor, which may be separate from the device, so that the membrane bodies attached thereto rotate in the continuous phase about the longitudinal axis of the shaft.
  • the disperse phase is pressed through the pores of the membrane body in the continuous phase, wherein the detachment of the droplets takes place as in the membrane technique described above.
  • the present device and associated method have particular advantages due to their structure and associated operation.
  • the required overflow velocity of the continuous phase across the membrane surface is already achieved by the rotation of the membrane body.
  • the attached to the shaft hollow membrane body are designed to exploit the above effect as a disc-shaped membrane hollow body through whose center of symmetry the shaft extends.
  • the individual disks preferably have the same disk diameter and are arranged at approximately constant spacing and parallel to one another on the shaft. This results in an approximately cylindrical rotational space, which can be enclosed by a cylindrically shaped housing.
  • the supply channel is not attached to the shaft as a separate channel.
  • the shaft is designed as a hollow shaft, so that it forms the feed channel itself.
  • the connection between the supply channel and the interior of the hollow membrane body is achieved via suitable openings of the hollow shaft or the supply channel and the membrane body at the corresponding attachment points of the membrane body on the shaft.
  • the present device can be used both for a discontinuous and for a continuous Production of emulsions are used.
  • the continuous phase is first introduced into the housing.
  • the membrane bodies are set in motion via the shaft and the dispersed phase is introduced under pressure into the membrane body.
  • a predetermined time interval which is sufficient for the preparation of the desired emulsion, it is withdrawn through the outlet opening and the whole process begins again.
  • the continuous phase is constantly through the inlet port fed and the emulsion constantly withdrawn through the outlet opening.
  • the pump required for this purpose only has to ensure the transport of the liquid medium from the inlet to the outlet opening.
  • the required overflow velocities across the surface of the membrane body are achieved by the rotation of the membrane body.
  • the number of membrane body as well as the dimensions of the membrane body and the housing as well as the pressure of the disperse phase in the membrane bodies and the residence time of the continuous phase in the housing selected by the skilled person to achieve the desired result depending on the liquid media used ,
  • the choice of materials of the membrane body and their separation limits can be used in addition to ceramic materials for the membrane body.
  • polymer materials or other inorganic materials such as metals, carbons, glasses, can be used.
  • the introduction of the disperse into the continuous phase can be improved by the choice of membrane materials with defined surface properties. It may be advantageous to provide the membrane surface hydrophilic, hydrophobic to oleophobic. This can be achieved by the choice of membrane material or by additional coatings even with inorganic materials.
  • the membranes themselves may be formed as nanofiltration membranes, ultrafiltration membranes or microfiltration membranes.
  • a suitable material is chosen, which is compatible with the liquid media used.
  • FIG. 1 shows schematically the operation of the membrane technique for the preparation of emulsions, as it is known from the prior art.
  • a tube membrane 12 is used, which is flowed through by a continuous phase 9.
  • the disperse phase 8 is pressed through the pores 13 of the tube membrane 12, so that 14 form droplets 15 on the inner membrane surface, which are entrained after reaching a certain droplet size of the continuous phase 9, so that at the outlet the tube membrane 12 is an emulsion 10 is present.
  • FIG. 2 shows an embodiment of a device according to the present invention which does not have such a high energy consumption to produce the emulsion.
  • the device consists of a housing 1 with an inlet opening 2 for the continuous phase 9 and an outlet opening 3 for the finished emulsion. Valves 16 are respectively provided at the inlet 2 and the outlet opening 3 in order to be able to interrupt the inflow or outflow of the continuous phase 9 or of the emulsion 10.
  • a rotatably drivable shaft 4 is formed in the housing, to which four disc-shaped membrane bodies 6 are fastened in the present example.
  • the shaft 4 is a hollow shaft which simultaneously forms the feed channel 5 for the disperse phase 8.
  • the supply channel 5 is connected to the attachment of the membrane discs 6 with the hollow shaft 4 with the hollow interior spaces of the membrane discs 6 formed as filter elements.
  • the hollow shaft 4 in this case passes through the center of symmetry of the individual membrane discs 6, so that they are driven to rotate about their axis of symmetry by the hollow shaft 4.
  • the housing 1 has an inner contour 7, which adapts to the contour of the membrane discs 6 and the hollow shaft 4, so that only small gaps between the inner contour 7 and the membrane bodies 6 and the hollow shaft 4 arise, as can be seen from the figure , These intermediate spaces 11 form the feed or emulsion space, through which the continuous phase 9 is guided past the surfaces of the membrane body 6.
  • the hollow shaft 4 is mounted via a corresponding bearing 17 within the housing 1.
  • the membrane discs 6 have a diameter of about 150 mm, the housing has a diameter and a height in the order of 20 cm.
  • the membrane discs themselves are formed of a ceramic material.
  • the disperse phase 8 is introduced under pressure, which is applied for example by a pump or a gas cushion generated by compressed air, through the supply channel 5 of the hollow shaft 4 in the membrane discs 6.
  • the continuous phase 9 is guided via the valve 16 and the inlet opening 2 into the emulsion space 11 of the housing 1.
  • the membrane discs are rotated by rotational drive of the shaft 4 in the continuous phase 9. This rotation causes an overflow of the membrane surfaces with the continuous phase 9, which is required for the detachment of the droplets of the disperse phase 8 from the surface of the membrane body 6.
  • the detachment mechanism takes place in the same way as in the conventional membrane technique of Figure 1.
  • the rotation of the shaft 4 takes place in such a way that overflow velocities of 2 to 5 m / s are achieved at the outermost regions of the membrane disks 6.
  • continuous production of the emulsion can also be achieved by continuously feeding the continuous phase 9 via the inlet opening 2 and continuously drawing off the emulsion 10 via the outlet opening 3 while the membrane disks 6 are driven in rotation.
  • both oil / water and water / oil emulsions and liposomes can be produced.
  • the device leads to a low heating of the emulsion during the manufacturing process, which is particularly advantageous when using heat-sensitive substances.
  • As well as known systems of the prior art can be carried out with the present device also a sterile operation without intermediate sterilization to the final product.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Colloid Chemistry (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Medicinal Preparation (AREA)
  • Polymerisation Methods In General (AREA)

Claims (5)

  1. Dispositif pour la préparation d'émulsions comprenant :
    - un boîtier (1) comportant une ouverture d'entrée (2) et une ouverture de sortie (3) pour une phase continue (9) d'un premier agent liquide,
    - un arbre (4), pouvant être entraîné en rotation dans le boîtier (1), sur ou dans lequel est formé un canal d'alimentation (5) pour une phase dispersée (8) d'un second agent liquide, et
    - plusieurs corps membranaires (6) en forme de disques écartés les uns des autres le long de l'arbre (4) et fixés à cet arbre de telle sorte que l'arbre passe par leur centre de symétrie (4), le canal d'alimentation (5) étant relié aux corps membranaires (6) au moyen de l'arbre (4) pour permettre l'apport de la phase dispersée dans les corps membranaires (6) via le canal d'alimentation (4),
    caractérisé en ce que
    les corps membranaires sont creux et l'espace séparant les corps membranaires (6) écartés les uns des autres est rempli par un contour intérieur (7) approprié du boîtier (1) en laissant un léger écart par rapport aux corps membranaires (6) et à l'arbre (4).
  2. Dispositif selon la revendication 1,
    caractérisé en ce que
    l'arbre (4) est un arbre creux formant le canal d'alimentation (5) pour la phase dispersée (8).
  3. Utilisation d'un dispositif selon la revendication 1 ou 2 pour la préparation d'une émulsion, selon laquelle une phase continue (9) est introduite dans le boîtier (1) via l'ouverture d'entrée (2) et une phase dispersée (8) est introduite sous pression dans les corps membranaires (6) via le canal d'alimentation (5) de l'arbre (4), les corps membranaires (6) étant soumis dans le boîtier (1), lors de l'amenée de la phase dispersée (8), à une rotation du fait de l'arbre (4) de sorte que la phase dispersée (8) s'échappe des corps membranaires (6) et se mêle à la phase continue (9) en produisant une émulsion (10).
  4. Utilisation selon la revendication 3,
    caractérisée en ce que
    l'ouverture d'entrée (2) et l'ouverture de sortie (3) du boîtier (1) sont refermées après l'introduction de la phase continue (9), la phase dispersée (8) est amenée sous l'effet de la rotation des corps membranaires (6) puis l'émulsion (10) est soutirée par l'ouverture de sortie (3) après un laps de temps défini.
  5. Utilisation selon la revendication 3,
    caractérisée en ce que
    la phase continue (9) est introduite en continu dans le boîtier (1) via l'ouverture d'entrée (2) et l'émulsion (10) produite est soutirée en continu par l'ouverture de sortie (3).
EP02011487A 2001-06-02 2002-05-24 Dispositif et procédé de préparation d'emulsions Expired - Lifetime EP1262225B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10127075A DE10127075C2 (de) 2001-06-02 2001-06-02 Vorrichtung und Verfahren zur Herstellung von Emulsionen mittels Membrankörpern
DE10127075 2001-06-02

Publications (3)

Publication Number Publication Date
EP1262225A2 EP1262225A2 (fr) 2002-12-04
EP1262225A3 EP1262225A3 (fr) 2003-05-02
EP1262225B1 true EP1262225B1 (fr) 2006-10-18

Family

ID=7687130

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02011487A Expired - Lifetime EP1262225B1 (fr) 2001-06-02 2002-05-24 Dispositif et procédé de préparation d'emulsions

Country Status (6)

Country Link
EP (1) EP1262225B1 (fr)
AT (1) ATE342765T1 (fr)
DE (2) DE10127075C2 (fr)
DK (1) DK1262225T3 (fr)
ES (1) ES2273944T3 (fr)
PT (1) PT1262225E (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10306259A1 (de) * 2003-02-14 2004-09-02 Ferrero Ohg Mbh Auf Milchbestandteilen basierende Süßware mit definierten Speisefettagglomeraten, sowie Verfahren und Vorrichtung zu ihrer Herstellung
DE102004040735B4 (de) * 2004-08-23 2006-11-23 ETH-Zürich, Institut für Lebensmittelwissenschaft, Laboratorium für Lebensmittelverfahrenstechnik Verfahren zur mechanisch schonenden Erzeugung von fein dispersen Mikro-/Nano-Emulsionen mit enger Tropfengrößenverteilung und Vorrichtung zum Durchführen des Verfahrens
DE102005008868A1 (de) * 2005-02-24 2006-08-31 Basf Ag Verfahren zur Herstellung einer wässrigen Polymerisatdispersion
MY149295A (en) 2006-07-17 2013-08-30 Nestec Sa Cylindrical membrane apparatus for forming foam
WO2010072230A1 (fr) * 2008-12-22 2010-07-01 Kmpt Ag Procédé et dispositif destiné à produire des émulsions et/ou suspensions
WO2010072237A1 (fr) * 2008-12-23 2010-07-01 Kmpt Ag Procédé et dispositif pour traiter des fluides
EP2260917A1 (fr) * 2009-05-29 2010-12-15 Novoflow GmbH Système de filtration et procédé pour optimiser la performance de filtration
US8771778B2 (en) 2010-09-09 2014-07-08 Frito-Lay Trading Company, Gmbh Stabilized foam
GB2505160A (en) * 2012-07-06 2014-02-26 Micropore Technologies Ltd Dispersion apparatus with membrane
US9393532B2 (en) 2013-02-27 2016-07-19 Dow Global Technologies Llc Swept membrane emulsification
EP3794013B1 (fr) 2018-05-17 2024-02-21 CSL Behring AG Procédé et système d'extraction de protéine

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2146867B2 (de) * 1971-09-20 1975-06-26 Hoechst Ag, 6000 Frankfurt Schelbendrehfiner
US4201691A (en) * 1978-01-16 1980-05-06 Exxon Research & Engineering Co. Liquid membrane generator
JPS58216726A (ja) * 1982-06-10 1983-12-16 Toshio Araki エマルジヨン流体の製造装置
JPH082416B2 (ja) * 1988-09-29 1996-01-17 宮崎県 エマルションの製造方法
DE4329077C1 (de) * 1993-08-30 1994-07-14 Chmiel Horst Konzentrisch angeordnete mikroporöse Zylinder zum Stoffaustausch in feinkörnigen Schüttungen, konzentrierten Suspensionen oder Emulsionen
US6386751B1 (en) * 1997-10-24 2002-05-14 Diffusion Dynamics, Inc. Diffuser/emulsifier
DE19823839A1 (de) * 1998-05-29 1999-12-09 Franz Durst Verfahren und Vorrichtung zum Mischen und Dispergieren mindestens zweier Phasen
GB9930322D0 (en) * 1999-12-22 2000-02-09 Univ Leeds Rotating membrane

Also Published As

Publication number Publication date
DE10127075C2 (de) 2003-04-10
EP1262225A2 (fr) 2002-12-04
DE50208468D1 (de) 2006-11-30
ES2273944T3 (es) 2007-05-16
DE10127075A1 (de) 2002-12-12
ATE342765T1 (de) 2006-11-15
DK1262225T3 (da) 2007-02-19
PT1262225E (pt) 2007-02-28
EP1262225A3 (fr) 2003-05-02

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