EP1781402B1 - Dispositif pour produire par une action mecanique douce des micro et nanoemulsions finement dispersees a distribution dimensionnelle etroite des gouttes - Google Patents

Dispositif pour produire par une action mecanique douce des micro et nanoemulsions finement dispersees a distribution dimensionnelle etroite des gouttes Download PDF

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Publication number
EP1781402B1
EP1781402B1 EP05776538A EP05776538A EP1781402B1 EP 1781402 B1 EP1781402 B1 EP 1781402B1 EP 05776538 A EP05776538 A EP 05776538A EP 05776538 A EP05776538 A EP 05776538A EP 1781402 B1 EP1781402 B1 EP 1781402B1
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EP
European Patent Office
Prior art keywords
filter fabric
accordance
membrane body
membrane
fluid phase
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.)
Not-in-force
Application number
EP05776538A
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German (de)
English (en)
Other versions
EP1781402A1 (fr
Inventor
Erich J. Windhab
Dr. Verena Eisner
Beat Troxler
Andreas Kurt DÜRIG
Fred-Rainer Grohmann
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.)
Eidgenoessische Technische Hochschule Zurich ETHZ
Processtech GmbH
Ion Bond AG
KINEMATICA AG
Original Assignee
Eidgenoessische Technische Hochschule Zurich ETHZ
Processtech GmbH
Ion Bond AG
KINEMATICA AG
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.)
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Publication date
Application filed by Eidgenoessische Technische Hochschule Zurich ETHZ, Processtech GmbH, Ion Bond AG, KINEMATICA AG filed Critical Eidgenoessische Technische Hochschule Zurich ETHZ
Publication of EP1781402A1 publication Critical patent/EP1781402A1/fr
Application granted granted Critical
Publication of EP1781402B1 publication Critical patent/EP1781402B1/fr
Not-in-force 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
    • 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
    • B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
    • 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
    • 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
    • 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
    • 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 device for mechanically gentle production of finely dispersed micro / nano-emulsions with a narrow droplet size distribution.
  • the production of finely dispersed emulsions is considered an important development goal for the food, pharmaceutical, cosmetics and chemical industries.
  • the reason for this is the possibility of having such emulsions with sufficient smallness of the disperse droplets entmischungsstabil to use and the extremely large inner interface for the adsorption of functional ingredients (eg., Active ingredients, flavors, dyes, etc.).
  • functional ingredients eg., Active ingredients, flavors, dyes, etc.
  • the disperse drops allow the construction of particle networks to which have a specific influence on the rheological properties of such emulsions.
  • Membrane emulsification processes are a new area for machine / apparatus manufacturers. Traditionally, rotor / stator dispersing systems and high-pressure homogenizers are used for fine emulsification. In these apparatus, the droplet is dispersed under extremely high mechanical stress of the disperse as well as the continuous phase. The present since about five years Membrane emulsification are very gentle from the conventional methods mentioned above, since the finely dispersed emulsion droplets are not produced by the tearing of larger drops, but these are formed and detached in their final size at the outlet openings of the membrane pores.
  • WO 01/45830-A1 is a cup-like structure previously known in which coaxially a tube with radially extending holes or holes dips, which is driven by a motor.
  • a tube with radially extending holes or holes dips which is driven by a motor.
  • the other phase is introduced and to be mixed by centrifugal force with the first in the cup-shaped housing phase to form an emulsion.
  • the finished mixture leaves through a radially disposed channel the cup-shaped housing.
  • a device for producing emulsions with a housing with inlet and outlet opening for a continuous phase of a first liquid medium is previously known, with a rotatably driven in the housing arranged shaft, formed on or in a supply channel for a disperse phase of a second liquid medium is.
  • the device has a plurality of opposite the outer diameter of the shaft considerably enlarged in diameter disk-shaped, hollow membrane body, which are formed as membrane discs and which are arranged in the longitudinal axis of the driving shaft with gap spacing and with gap distance between these membrane bodies arranged ridge-shaped housing parts.
  • the shaft is concentric with the membrane discs, with the feed channel over the shaft the interior of the individual membrane body is connected to allow the supply of the disperse phase via the supply channel in the disk-shaped membrane body.
  • the continuous phase is introduced radially into the gap distance between the radial housing webs and the various membrane disks and coaxially exits the housing after it has peeled from the membrane discs emerging droplets of the disperse phase and mixed with these to form an emulsion.
  • the invention has for its object to provide a device for mechanically gentle production of finely dispersed micro / nano-emulsions with narrow droplet size distribution.
  • the gentle detachment of smaller drops and their more efficient further dispersion after detachment is possible due to a shear flow superimposed Dehnströmungsanteile on the rotating membrane surface, as is the case with realization of pure shear flows of the case.
  • Emulsion droplets are produced in the device according to the invention on the surface of a pore-permeated membrane or a filter fabric by pressing a first fluid phase through these pores and removing the droplets from the membrane surface by rotating them in a second with the first immiscible fluid phase takes place.
  • the detachment of the fluid droplets from the membrane surface is effected by tangential and normal stresses acting on them, supported by additional centrifugal forces.
  • the preferred use of membranes with defined pore spacing compared to pore diameter x ( ⁇ 2x) is additionally conducive to the generation of a narrow droplet size distribution in the emulsion produced.
  • the membrane overflow according to the invention which is realized with additionally efficient expansion flow fractions, permits the production of significantly smaller droplet diameters with a comparable pore diameter.
  • the emulsion droplet production according to the invention offers the advantage of significantly reduced mechanical stress at comparable diameters of the droplets produced. This has advantages in terms of preserving native properties of functional content components, such as proteins in the droplets or at their interfaces.
  • the device according to the invention allows the simple modification and adaptation of the expansion flow overflow characteristic of the membrane according to the invention with regard to the proportion of the expansion flow to the total flow by varying the eccentricity of the rotating diaphragm cylinder and / or easily exchanged flow installations.
  • the inventive device is very compact, since the membrane body can be arranged in the housing with a narrow gap distance to the inner wall.
  • 4 denotes disperse drops and 5 denotes a membrane or filter fabric body, while 6 represents a cylinder body designed as a membrane cylinder.
  • a hollow shaft formed rotary shaft is designated, which has an inner, centrally arranged bore 8.
  • the shaft 7 is sealed by a dynamic mechanical seal 9.
  • the bore 8 opens into an interior 10 of the filter fabric or membrane body 5.
  • a conical component is arranged, which opens into an outlet connection 12.
  • the conical component 11 and the outlet connection 12 form part of a housing 18.
  • a disperse fluid phase is supplied from a container, also not shown, by means of a motor-driven pump (not shown).
  • the emulsion 14 leaves the housing 18 via the outlet connection 12.
  • the filter fabric or membrane body 5 is eccentric, with defined adjustable eccentricity, to the housing 18, respectively.
  • a flow installation (eg web 15) is arranged in the gap 3, which extends in the direction of the longitudinal axis 16 of the housing 18.
  • the web 15 may also be helical or part of a spiral. It is also possible to provide within the gap 3 a plurality of such webs 15, spirals or helically extending ridges 3 of different cross-sectional geometry.
  • the diametrically oppositely directed arrows 17 are intended to indicate the approximately radially directed flow direction of the disperse fluid phase 13 with respect to the filter fabric or membrane body 5.
  • Fig. 5 is a corresponding number sum distribution Q 0 (x) with entry of the characteristic droplet sizes x 90,0 and x 10,0 whose ratio (x 90,0 / x 10,0 ) is used as a suitable measure for the droplet size distribution width, the representation for centric arrangement (Z) and eccentric arrangement (EZ) (and and Dehnströmanteile) were illustrated.
  • the disperse fluid phase 13 is pressed by means of the not shown, motor-driven pump via the provided with an inner bore 8 and thus designed as a hollow shaft rotating shaft 7 into the interior 10 of the rotating diaphragm cylinder body 6.
  • the shaft 7 is dynamically sealed against the housing 18 by means of the mechanical seal 9. From there, the disperse fluid phase 13 passes through the membrane 5 applied to the cylinder body surface and forms the disperse drops 4 on its outside.
  • the continuous fluid phase 1 is passed through the port 2 in the cylindrical housing 18 and flows through the gap 3 between the rotating membrane or filter fabric body 5 and housing 18 in the axial direction.
  • the disperse drops 4 formed on the membrane surface are flown.
  • the intensity of the flow is determined by the circumferential speed of the membrane or filter cloth body or cylinder 6, the gap width 3 and the eccentricity or flow attachments (eg web (s), pins, knife / scraper) attached to the outer cylinder wall and the housing 18 fixed.
  • a mixed shear / elongation flow is formed which has improved dispersing properties.
  • the rotational flow is defined with disturbing flow installations (for example web 15), preferably attached to the inner wall of the housing.
  • Such flow internals eg web 15
  • the mixture of disperse drops 4 and continuous fluid phase 1, the emulsion 14, is formed at the exit from the gap 3 in an outlet geometry, which preferably consists of a conical component 11 and an outlet connection 12.
  • CPDN membrane Controlled Pore Distance Membrane

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Colloid Chemistry (AREA)
  • Cosmetics (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Claims (23)

  1. Dispositif permettant de fabriquer, mécaniquement en douceur, des micro-émulsions/nanoémulsions finement dispersées dont les tailles de gouttes sont réparties dans une fourchette étroite, les gouttes (4) étant générés par un corps à textile filtrant ou corps à diaphragme (5) doté de pores dans lequel une première phase fluide (13) est déplacée à travers ces pores, notamment pressée, et le mouvement d'éloignement (l'enlèvement) des gouttes (4) de la surface à textile filtrant ou surface à diaphragme ayant lieu du fait de leur mouvement propre dans une deuxième phase fluide (1) non miscible avec la première, avec génération de parts de flux de cisaillement en superposition et de flux de dilatation marqués dans l'interstice entre le cylindre à diaphragme et la paroi du carter, de sorte qu'un corps à textile filtrant et corps à diaphragme (5) de préférence symétrique en rotation est agencé mobile par motorisation autour de son axe longitudinal dans un carter (18) de capotage présentant un interstice (3) d'ouverture variable.
  2. Dispositif selon la revendication 1, caractérisé en ce que le corps textile filtrant ou le corps à diaphragme (5) a la forme d'un cylindre.
  3. Dispositif selon la revendication 1, caractérisé en ce que le corps textile filtrant ou le corps à diaphragme (5) a la forme d'un disque.
  4. Dispositif selon la revendication 1, caractérisé en ce que la paroi intérieure du carter (18), laquelle limite l'interstice (3), et le corps textile filtrant ainsi que le corps à diaphragme (5) sont agencés de façon mutuellement excentrique.
  5. Dispositif selon la revendication 1, caractérisé en ce que dans l'interstice (3) sont agencées une ou plusieurs nervures (15) officiant de génératrice(s) des parts de flux de dilatation.
  6. Dispositif selon la revendication 5, caractérisé en ce que la nervure concernée (15) s'étend dans le sens de l'axe longitudinal du carter (18) et du corps à textile filtrant et du corps à diaphragme (5).
  7. Dispositif selon les revendications 5 ou 6, caractérisé en ce que la nervure concernée (15) est rectiligne, ou configurée en spirale ou en spirale hélicoïdale.
  8. Dispositif selon la revendication 5 ou l'une des revendications suivantes, caractérisé en ce que la nervure concernée (15) est agencée contre la paroi intérieure du carter (18).
  9. Dispositif selon la revendication 1 ou l'une des revendications suivantes, caractérisé en ce que la vitesse circonférentielle du corps à textile filtrant ou corps à diaphragme (5) entraînable en rotation est comprise entre 1 m/s et 50 m/s.
  10. Dispositif selon la revendication 1 ou l'une des revendications suivantes, caractérisé en ce que la vitesse axiale du flux couvrant le corps cylindrique à textile filtrant ou à diaphragme (5) est réglable, notamment pilotable et régulable, par la phase fluide continue (1), indépendamment de la vitesse circonférentielle du corps textile filtrant ou corps à diaphragme (5).
  11. Dispositif selon la revendication 1 ou l'une des revendications suivantes, caractérisé en ce que la phase fluide dispersée (13) est amenée via un arbre creux (7) à ce corps à textile filtrant ou corps à diaphragme (5) relié avec cet arbre, et qu'elle peut être refoulée à travers ce dernier sous la pression exercée par une pompe, de sorte que des gouttes de fluide (4) dispersées soient fabricables à la surface du corps à textile filtrant ou corps à diaphragme (5).
  12. Dispositif selon la revendication 1 ou l'une des revendications suivantes, caractérisé en ce que le mouvement propre du corps à textile filtrant ou corps à diaphragme (5) est réglable via un dispositif de pilotage ou de régulation.
  13. Dispositif selon la revendication 1 ou l'une des revendications suivantes, caractérisé en ce que le mouvement propre du corps à textile filtrant ou corps à diaphragme (5) est exécutable via un programme d'ordinateur.
  14. Dispositif selon la revendication 1, caractérisé en ce que le corps à textile filtrant ou corps à diaphragme (5) peut se déplacer en rotation selon une vitesse constante réglable.
  15. Dispositif selon la revendication 1, caractérisé en ce que le corps à textile filtrant ou corps à diaphragme (5) peut se déplacer en rotation selon une vitesse en oscillation périodique.
  16. Dispositif selon la revendication 1, caractérisé en ce que le corps à textile filtrant ou corps à diaphragme (5) est traversé continuellement ou de façon pulsée par une phase fluide (13) dispersée.
  17. Dispositif selon la revendication 1, caractérisé en ce que la phase fluide continue (1) ou un autre fluide non miscible avec la phase fluide (13) dispersée traverse brièvement le système à textile filtrant ou à diaphragme poreux avant que le corps à textile filtrant ou le corps à diaphragme (5) ne soit traversé par la phase fluide dispersée (13), ceci dans le but que la phase appliquée en premier contre les parois du textile filtrant ou les parois poreuses du diaphragme du corps à textile filtrant ou corps à diaphragme (5) repousse la phase fluide (13) dispersée.
  18. Dispositif selon la revendication 1 ou 14, caractérisé en ce que le mouvement du corps à textile filtrant ou corps à diaphragme (5) permet d'ajuster des tensions de cisaillement et/ou de dilatation prédéterminées et définies dans les gouttes d'émulsion (4) formées à la surface du textile filtrant ou la surface à diaphragme.
  19. Dispositif selon la revendication 1, caractérisé en ce que le corps à textile filtrant ou corps à diaphragme (5) est baigné en plus par un flux en superposition perpendiculaire au sens circonférentiel du mouvement de rotation, c'est-à-dire dans le sens radial en présence d'un corps à textile filtrant ou corps à diaphragme en forme de disque, et dans le sens axial en présence d'un corps à textile filtrant ou corps à diaphragme (5) en forme de cylindre.
  20. Dispositif selon la revendication 1, caractérisé en ce que la phase fluide (13) traversant le corps à textile filtrant ou corps à diaphragme (5) représente de son côté une émulsion et qu'ainsi, après que les gouttes formées (4) se soient éloignées de la surface du textile filtrant ou de la surface du diaphragme, une double émulsion du type eau/huile/eau ou huile/eau/huile se forme dans une autre phase fluide.
  21. Dispositif selon la revendication 1, caractérisé en ce que la phase fluide (1) guidée le long de la surface du corps à textile filtrant ou corps à diaphragme (5) représente de son côté une suspension qui, après l'enlèvement des gouttes (4), forme un système suspension/émulsion dans une autre phase fluide enveloppante.
  22. Dispositif selon la revendication 1 ou l'une des revendications suivantes, caractérisé en ce que le mécanisme d'entraînement motorisé affecté à la pompe refoulant la phase fluide (13) peut être mû de façon intermittente (pulsée) selon un programme prédéfini.
  23. Dispositif selon la revendication 1 ou l'une des revendications suivantes, caractérisé en ce que le mécanisme d'entraînement motorisé affecté à la pompe refoulant la phase dispersée (1) peut être mû de façon intermittente (pulsée) selon un programme prédéfini.
EP05776538A 2004-08-23 2005-08-19 Dispositif pour produire par une action mecanique douce des micro et nanoemulsions finement dispersees a distribution dimensionnelle etroite des gouttes Not-in-force EP1781402B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004040735A DE102004040735B4 (de) 2004-08-23 2004-08-23 Verfahren zur mechanisch schonenden Erzeugung von fein dispersen Mikro-/Nano-Emulsionen mit enger Tropfengrößenverteilung und Vorrichtung zum Durchführen des Verfahrens
PCT/EP2005/008980 WO2006021375A1 (fr) 2004-08-23 2005-08-19 Procede pour produire par une action mecanique douce des micro et nanoemulsions finement dispersees a distribution dimensionnelle etroite des gouttes et dispositif pour la mise en oeuvre dudit procede

Publications (2)

Publication Number Publication Date
EP1781402A1 EP1781402A1 (fr) 2007-05-09
EP1781402B1 true EP1781402B1 (fr) 2008-02-27

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EP05776538A Not-in-force EP1781402B1 (fr) 2004-08-23 2005-08-19 Dispositif pour produire par une action mecanique douce des micro et nanoemulsions finement dispersees a distribution dimensionnelle etroite des gouttes

Country Status (6)

Country Link
US (1) US8267572B2 (fr)
EP (1) EP1781402B1 (fr)
JP (1) JP4852042B2 (fr)
AT (1) ATE387255T1 (fr)
DE (2) DE102004040735B4 (fr)
WO (1) WO2006021375A1 (fr)

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DE10307568B4 (de) * 2003-02-22 2007-08-16 ETH-Zürich, Institut für Lebensmittelwissenschaft, Laboratorium für Lebensmittelverfahrenstechnik Verfahren zum Herstellen einer Membran mit Membranlöchern und nach diesem Verfahren hergestellte Mikro-/Nanomembran
DE602004009681T2 (de) * 2003-05-16 2008-08-14 Velocys, Inc., Plain City Verfahren zur erzeugung einer emulsion durch verwendung einer mikrokanalverfahrentechnologie
US7485671B2 (en) * 2003-05-16 2009-02-03 Velocys, Inc. Process for forming an emulsion using microchannel process technology
US7396550B2 (en) * 2003-06-05 2008-07-08 Angel Michael G Time released nutritional product and method of manufacture

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US8267572B2 (en) 2012-09-18
DE502005003021D1 (de) 2008-04-10
JP4852042B2 (ja) 2012-01-11
WO2006021375A1 (fr) 2006-03-02
DE102004040735A1 (de) 2006-03-09
ATE387255T1 (de) 2008-03-15
EP1781402A1 (fr) 2007-05-09
DE102004040735B4 (de) 2006-11-23
US20110038901A1 (en) 2011-02-17
JP2008510607A (ja) 2008-04-10

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