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WO2005056169A1 - Procede et dispositif de production d'emulsions monodispersees - Google Patents

Procede et dispositif de production d'emulsions monodispersees Download PDF

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Publication number
WO2005056169A1
WO2005056169A1 PCT/EP2004/014005 EP2004014005W WO2005056169A1 WO 2005056169 A1 WO2005056169 A1 WO 2005056169A1 EP 2004014005 W EP2004014005 W EP 2004014005W WO 2005056169 A1 WO2005056169 A1 WO 2005056169A1
Authority
WO
WIPO (PCT)
Prior art keywords
capillary
phase
continuous phase
capillaries
dispersed
Prior art date
Application number
PCT/EP2004/014005
Other languages
German (de)
English (en)
Inventor
Thomas Melin
Rainer Gruber
Jens Hoppe
Bernd Klinksiek
Olaf Behrend
Martin Steinbeck
Olaf Stange
Original Assignee
Rwth Aachen
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 Rwth Aachen filed Critical Rwth Aachen
Publication of WO2005056169A1 publication Critical patent/WO2005056169A1/fr

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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
    • B01F23/41—Emulsifying
    • B01F23/4105—Methods of emulsifying
    • 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
    • B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
    • B01F23/451—Mixing liquids with liquids; Emulsifying using flow mixing by injecting one liquid into another
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
    • B01F25/31421—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction the conduit being porous

Definitions

  • the invention relates to a method and a device for producing monodisperse emulsions.
  • Emulsions i.e. Liquid-liquid dispersions are used in many areas as end or intermediate products.
  • the drop size of the emulsion often has a decisive influence on the relevant quality characteristics. In many cases, only a certain average drop size is sufficient;
  • the droplet size distributions of typical emulsions produced using conventional apparatus and processes generally extend over a range of one to two powers of ten.
  • Emulsions are usually produced by distributing the disperse phase in the continuous phase using mechanical energy and crushing it to the desired average drop size and then stabilizing the system with suitable additives.
  • apparatuses operating on this principle are stirred tanks, continuously operated rotor-stator arrangements or high-pressure nozzle dispersion systems.
  • the group of the latter methods has the disadvantage that high proportions of disperse phase can generally only be achieved in the range of low throughputs.
  • high-pressure homogenizers are particularly suitable for producing very fine-particle emulsions in the range below 10 ⁇ m.
  • Nozzle dispersing systems are therefore not directly comparable with the subject matter of the invention (compare SCHULTZ, S .; WAGNER, G .; ULRICH, J .: High pressure homogenization as a process for the production of emulsions. Chem. Ing. Techn., 74 (7); 2002. 901-909).
  • Drops with a very narrow drop size distribution can be produced by laminar dripping.
  • Drop sizes of 0.5 to 3 mm are used in technical systems, e.g. generated when prilling (sprayer stare).
  • the lower drop limit is limited on the one hand by the throughput, which decreases with the third power of the drop size at a constant drop frequency, and on the other hand by the bore diameter of the nozzle plate, which must be approximately equal to half the drop diameter. Bores below 0.1 to 0.5 mm tend to become blocked, especially when working with pure viscous suspensions rather than pure solutions.
  • Such draining systems which are usually can be improved by vibration exciters with regard to the uniformity of the drop sizes as well as the drop formation frequency, e.g. van Fa. Brace (http://www.brace.de/index.sh.tml7deutschc06i26). Rieter (http://www.rieter-automatik.de/deutsch/Granuliersysteme/link2html), The Technology Partnership plc (Hertfordshire, UK), Inotech (http://www.motech.ch/products.htm , http: // www.inotech.ch index.htrh), among others
  • Emulsification with membranes and microstructured systems In membrane emulsification, the phase to be dispersed flows through the pores of a microporous membrane into the continuous phase. Individual drops are formed at the pore mouth, which, for example, by periodically overflowing the membrane.
  • specially manufactured, microstructured components instead of the mostly irregularly structured membranes, specially manufactured, microstructured components with defined, uniform pore dimensions are used.
  • Narrow droplet size distributions can therefore only be produced using components with correspondingly narrow pore sizes (see: SCHR ⁇ DER, V .: Production of oil-in-water emulsions with microporous membranes. Shaker Verlag, Achen; 199. KOBAYASHI, I .; NAKAJIMA, M .; CHUN, K .; KIKUCHI, Y .; FUJITA, H .: Silicon array of elongated through-holes for monodisperse emulsion droplets. AIChE J., 48 (8); 2002.1639-1644).
  • porous hollow fibers are used which are flowed through axially by a liquid, radially through the porous wall by a second, immiscible liquid.
  • the first liquid is distributed in the form of drops in the inside of the fibers and an emulsion is formed.
  • a large pre-emulsion flows through the capillaries, in which the mean size of the drops is of the order of the inside diameter of the capillary.
  • the invention relates to a method for producing finely divided monodisperse dispersions, in particular of the oil-in-water emulsion type, with the steps
  • the surface of the capillary is wettable by the continuous phase.
  • the capillary is particularly preferably a hollow fiber.
  • the pressure difference across the membrane wall is at least 150 hPa.
  • the continuous phase is preferably an aqueous phase, particularly preferably selected from the series: water, aqueous solutions of inorganic and organic salts, acidic or basic aqueous solutions and aqueous polymer solutions.
  • the phase to be dispersed is preferably an oil phase, particularly preferably selected from the series: aliphatic or aromatic hydrocarbons, in particular long-chain alkanes and alcohols, and organically dissolved monomers or polymers.
  • the invention also relates to a device for producing monodisperse emulsions and in particular for carrying out the method according to the invention described above, at least comprising a feed for the continuous phase and a capillary, preferably a bundle of capillaries, in particular arranged in parallel, with a membrane wall permeable to the phase to be dispersed a supply space for the continuous phase surrounding the capillary, which can be pressurized with a continuous phase and a collecting container into which the ends of the capillaries open.
  • a device is preferred which is characterized in that the capillary inner wall is designed to be wettable by the continuous phase.
  • a preferred form of the device is characterized in that the ends of the capillaries in the collecting container have an oblique cut with a cut angle of at least 45 ° to the capillary cross-section.
  • the capillary hollow fibers are particularly preferably made of polyethersulfone (PES).
  • the drop sizes of the emulsions emerging at the fiber or capillary orifices are very narrowly distributed.
  • the principle can also be implemented with high product throughputs. Even concentrated emulsions with disperse phase components of more than 50% can be produced in a simple manner.
  • Hollow fiber or capillary membranes arranged in parallel in a so-called module are flowed through on the lumen side (inside the fiber) with the phase to be dispersed.
  • the membrane material is selected so that it is preferably wetted by the continuous phase. This is pressed from the jacket space through the porous membrane wall into the interior of the fiber and displaces the phase to be dispersed from the membrane wall.
  • the incoming liquid disrupts the smooth surface of the strand, corrugates it and continues to break in the strand of the phase to be dispersed until it finally disintegrates (view A). If there is sufficient open-pore fiber length (b), the constriction and cutting continues until the resulting structures have reached a more stable shape (eg drops or capsules). The droplet formation takes place completely in the fiber.
  • the drops After exiting the fiber openings, the drops enter a type of collecting container (area c). At the same time, the continuous phase flows together with the drops into the collecting container, which is an additional advantage of this dispersion process. Because the drops are already surrounded within the fibers with a sufficiently continuous phase, this no longer has to be delivered from the outside when the dispersion rises in area c. In this way, a narrowing of the ascending drop strand and the associated coalescence of drops, as can be observed in conventional methods, can be avoided.
  • the collecting container offers the possibility of adding an additional process step such as a polymerization (e.g. ion exchange balls), a crosslinking reaction or a precipitation bath.
  • a polymerization e.g. ion exchange balls
  • a crosslinking reaction e.g. a crosslinking reaction
  • a precipitation bath e.g. a polymerization (e.g. ion exchange balls), a crosslinking reaction or a precipitation bath.
  • the principle of the method is illustrated by means of a system in which the phase to be dispersed has the lower density and therefore rises upwards. In the same way, however, narrowly disperse drops of a denser medium can be generated in a lighter continuous phase. These would then move down through the module and be collected in a container located below the hollow fibers.
  • This (fiber) section through which the phase to be dispersed flows first, can also be referred to as an equalization section or resistance section.
  • the fibers are resin-coated here, on the other hand, a constructive measure is to ensure that the phase to be dispersed is evenly distributed over the individual fibers. Different volume flows and thus unequal operating states within each membrane can lead to an expansion of the droplet size distribution. Backflows must be avoided of the continuous phase, which would lead to only single-phase flow through these fibers and to a mixing of both phases even before entering the module.
  • the desired pre-pressure loss can be set by suitable choice of material (permeability).
  • permeability permeability
  • FIG. 3, variant A An extension of the resin-coated fiber area or the inlet section is also conceivable (FIG. 3, variant A).
  • the flow through the interior of the fiber creates the necessary pre-pressure loss before entering the dispersion section (b). If the fiber openings are closed as shown in FIG. 3 (variant B), a flow resistance can be set by guiding the phase to be dispersed through the porous membrane wall.
  • FIG. 5 A photo of this operating point is shown in the following FIG. 5.
  • the drop sizes were determined using a stroboscope. This resulted in an average drop diameter of approximately 500 ⁇ m.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Colloid Chemistry (AREA)

Abstract

L'invention concerne un procédé et un dispositif de production d'émulsions monodispersées. Le dispositif comprend une amenée (1) de la phase continue, et un capillaire (2), de préférence, un faisceau de capillaires et, principalement, de capillaires disposés parallèlement entre eux (2), une paroi à membrane, perméable à la phase à disperser (4), un espace d'amenée (3) entourant les capillaires, pour la phase continue (5), lequel est sollicité à la pression (5), et un récipient collecteur (6) à l'intérieur duquel débouchent les extrémités des capillaires.
PCT/EP2004/014005 2003-12-10 2004-12-09 Procede et dispositif de production d'emulsions monodispersees WO2005056169A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10357564A DE10357564A1 (de) 2003-12-10 2003-12-10 Verfahren und Vorrichtung zur Erzeugung monodisperser Emulsionen
DE10357564.2 2003-12-10

Publications (1)

Publication Number Publication Date
WO2005056169A1 true WO2005056169A1 (fr) 2005-06-23

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PCT/EP2004/014005 WO2005056169A1 (fr) 2003-12-10 2004-12-09 Procede et dispositif de production d'emulsions monodispersees

Country Status (2)

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DE (1) DE10357564A1 (fr)
WO (1) WO2005056169A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006136555A1 (fr) * 2005-06-21 2006-12-28 Basf Aktiengesellschaft Procede de production d'une dispersion aqueuse de polymere

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997036674A1 (fr) * 1996-03-29 1997-10-09 Disperse Technologies Limited Dispersion de phases immiscibles
WO2003014196A1 (fr) * 2001-08-03 2003-02-20 Akzo Nobel N.V. Procede de preparation de dispersions

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997036674A1 (fr) * 1996-03-29 1997-10-09 Disperse Technologies Limited Dispersion de phases immiscibles
WO2003014196A1 (fr) * 2001-08-03 2003-02-20 Akzo Nobel N.V. Procede de preparation de dispersions

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006136555A1 (fr) * 2005-06-21 2006-12-28 Basf Aktiengesellschaft Procede de production d'une dispersion aqueuse de polymere

Also Published As

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DE10357564A1 (de) 2005-07-21

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