EP2049235B1 - Dispositif d'émulsification et procédé de formation d'une émulsion - Google Patents

Dispositif d'émulsification et procédé de formation d'une émulsion Download PDF

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Publication number
EP2049235B1
EP2049235B1 EP07786556A EP07786556A EP2049235B1 EP 2049235 B1 EP2049235 B1 EP 2049235B1 EP 07786556 A EP07786556 A EP 07786556A EP 07786556 A EP07786556 A EP 07786556A EP 2049235 B1 EP2049235 B1 EP 2049235B1
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EP
European Patent Office
Prior art keywords
channel
emulsifying device
injection
dispersed
phase
Prior art date
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EP07786556A
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German (de)
English (en)
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EP2049235A1 (fr
Inventor
Stephan Herminghaus
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Max Planck Gesellschaft zur Foerderung der Wissenschaften eV
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Max Planck Gesellschaft zur Foerderung der Wissenschaften eV
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30—Micromixers
    • B01F33/301—Micromixers using specific means for arranging the streams to be mixed, e.g. channel geometries or dispositions
    • B01F33/3012—Interdigital streams, e.g. lamellae
    • 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
    • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B01F25/3141—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit with additional mixing means other than injector mixers
    • 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
    • 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
    • B01F25/31424—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 with a plurality of perforations aligned in a row perpendicular to the flow direction
    • 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
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • 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
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4336—Mixers with a diverging cross-section

Definitions

  • the invention relates to an emulsifying device for forming an emulsion having a continuous and at least one dispersed phase, in particular an emulsifying device having a channel (or gap) adapted to receive laminar, flowing liquid filaments of the different phases and having a channel widening on which the at least one dispersed phase decomposes into individual drops.
  • the invention further relates to a process for forming an emulsion having a continuous phase and at least one dispersed phase, in particular a process for producing a mixed emulsion having a plurality of dispersed phases.
  • the invention relates to an emulsifying device and an emulsifying method having the features of the preambles of the independent claims.
  • a conventional emulsifier 100 'for forming a continuous phase emulsion and at least one dispersed phase derived from C. Priest et al. in Applied Physics Letters (Vol. 88, 2006, 024106-01 ) is schematically shown in FIG FIG. 11 illustrated.
  • the emulsifying device 100 ' comprises a dispersion region 10' which is formed as part of a channel 20 'in the interior of a fluidic microsystem.
  • the channel 20 ' is connected to a supply line 30' for supplying the continuous phase 2 'and to a injection line 40' for supplying the dispersed phase 3 '.
  • Bottom and top walls of the channel 20 ' have such a small vertical distance that the immiscible liquids of the continuous and dispersed phases in the channel 20' as thin filaments flow side by side.
  • the interface which separates the two liquids extends between the bottom and top walls.
  • the continuous and dispersed phases form a dynamic stable, laminar flow.
  • the channel 20' widens stepwise.
  • An edge 11 ' is provided at which the thread-like liquid flows become unstable and disintegrate into individual drops.
  • the dispersed phase 3' is distributed drop-wise in the continuous phase 2 ', so that downstream of the dispersion region 10' the phases 2 ', 3' in the channel 20 'continue to flow as emulsion 1'.
  • the conventional emulsifying device 100 ' according to FIG. 11 has the disadvantage that the dispersion region 10 'with the widening channel 20' is located inside the microsystem. The droplets of the dispersed phase are generated substantially serially. As a result, with the conventional emulsifying device 100 ', only small amounts of emulsion can be produced, which are too low for practical applications, for example in liquid phase processing technology. In order to increase the amount of emulsion, a large number of emulsifying devices 100 ' would have to be combined, which, however, represents an unacceptably high expenditure on equipment.
  • a solution to this problem could be achieved with a mixture of the different liquids, based not on the phenomenon of turbulence, but on a common emulsification.
  • instantaneously a mixed emulsion with a certain mixing ratio can be set, which is then constant for the entire duration of the reaction.
  • the initially existing phase boundaries in the emulsion can be interrupted by an external influence, such as a microwave field or an electrical voltage, in order to obtain a defined starting time for the start of the reaction of the liquids.
  • the conventional emulsifier 100 'in addition to the mentioned problem of low emulsion yield additionally has the disadvantage that it is only limited suitable for the preparation of a mixed emulsion. So far, in particular, no way has been published, as with the conventional emulsifier 100 'a mixed emulsion could be produced.
  • the invention has for its object to provide an improved emulsifying device, with which the disadvantages of the conventional emulsification techniques are overcome.
  • the invention is further based on the object of providing an improved emulsification process which overcomes the disadvantages of conventional emulsification techniques.
  • the emulsifier and the emulsification process should in particular have a broader field of application and be particularly suitable for the preparation of mixed emulsions.
  • the invention is based on the general technical teaching to provide an emulsifier for forming a continuous phase emulsion and at least one dispersed phase having a dispersion area for forming the emulsion by decomposing laminar flows of the continuous and the at least one dispersed phase , wherein a channel for receiving the laminar flows and a plurality of injection bores are provided, through which the at least one dispersed phase is injectable into the channel, and the dispersion region is formed by a gap mouth of the channel, which directly into a free environment of Emulgerer wisdom opens.
  • the combination according to the invention of a multiplicity of injection bores opening into the channel with a dispersion region formed by a channel end advantageously provides a compact emulsion source with which an emulsion of practically interesting rates and volumes can be provided directly in a reaction vessel.
  • the injection wells allow numerous liquid filaments to be formed from a single or multiple, e.g. B. two different dispersed phases in the channel are formed simultaneously and flow to the dispersion region. Unlike conventional serial emulsion production, parallel emulsion production is enabled.
  • the invention is based on the general technical teaching of providing an emulsification process in which the continuous phase and the at least one dispersed phase in the form of a multiplicity of laminar liquid filaments flowing from one channel at a split mouth into a free environment escape.
  • the emulsifying device contains a supply line for feeding the continuous phase into the channel.
  • the supply line has, at least adjacent to the channel, a straight direction with which an axial reference direction (z-direction) of the emulsifying device is determined.
  • the output of the emulsion from the emulsifying means may also be parallel to the axial reference direction (first embodiment of the invention) or in a direction other than the axial reference direction, particularly in a plane perpendicular to the axial reference direction, i. H. in a radial reference direction (x-direction) (second embodiment of the invention).
  • the emulsifying device according to the invention further comprises at least one injection line for feeding the dispersed phase into the channel. From each injection line, the dispersed phase is distributed through the injection wells in the channel.
  • the term "channel” or “gap” generally refers to a volume area between the injection wells and the dispersion area bounded by walls having such a small vertical distance that fluids injected through the injection wells form laminar flows.
  • the terms "continuous phase” and “dispersed phase” generally refer to liquids herein.
  • the liquid of the dispersed phase reactant, eg aqueous solution
  • carrier liquid eg an oil
  • environment of the emulsifying device refers to an area adjacent to the gap mouth of the channel, in which the emulsion can freely spread in at least two spatial directions.
  • the gap mouth has a curved Mouth history, so that advantageously the space density and thus the yield of the emulsion formation can be increased.
  • the dispersion region may extend in the reaction vessel for receiving the emulsion with a curved perpendicular to the axial extent of the emulsifying edge, the length of which is greater than would be the case with a straight course of the mouth.
  • Particularly preferred is an endless gap mouth with a closed mouth course, for example provided with a circular mouth course (annular gap). If the gap mouth of the channel is circular, there may be advantages for adjusting the exit of the emulsion in the axial or radial direction relative to the axial reference direction of the emulsifying device.
  • two injection lines for supplying the at least one dispersed phase are provided in the channel, each having a plurality of injection holes.
  • the injection holes open in opposite, z. B. upper and lower side walls in the channel. This simplifies the feeding of a dispersed phase with a high filament density in the channel and / or the separate feeding of different dispersed phases into the channel.
  • the mouths of the injection holes in the channel are distributed transversely to the flow direction in the channel so that from each injection hole a laminar remplisstechniksfilament can be formed to the gap mouth of the channel.
  • the at least one dispersed phase is distributed over the channel in the transverse direction thereof with the injection bores.
  • the two injection lines are provided for supplying various dispersed phases in the channel.
  • the injection lines are connected to separate reservoirs of a Fluidik adopted containing the dispersed phases.
  • the emulsifying device can thus be used for mixing the dispersed phases.
  • the injection bores have funnel-shaped injection openings, via which the injection line (s) is (are) connected to the injection bores.
  • the flow resistance during the supply of the at least one dispersed phase is thus reduced.
  • the funnel-shaped injection openings of adjacent injection bores can be connected by a groove, for example an annular groove.
  • the emulsion may advantageously be dispensed into a reaction vessel in a single direction.
  • the injection bores preferably run in the radial direction, that is to say perpendicular to the axial reference direction of the emulsifying device.
  • the at least one injection line and the supply line are arranged coaxially relative to one another, advantages for a compact construction of the emulsifying device can result.
  • the emulsifying device can advantageously have an outer shape of a cylinder, in which the injection line and the supply line extend axially and at the free end (front side) of the dispersion region is formed.
  • the channel extending to the dispersion region is aligned in the radial direction, that is, perpendicular to the axial reference direction of the emulsifying device (second embodiment of the invention)
  • advantages may be related by radially discharging the emulsion in different directions result in the emulsifier.
  • the channel extends in the radial direction from the supply line to an inner or outer peripheral edge of the emulsifying device.
  • the injection bores may advantageously be aligned parallel to the axial reference direction of the emulsifying device.
  • the channel is particularly preferably formed as a planar gap between two plates, which extend in the radial direction, that is perpendicular to the axial reference direction of the emulsifying.
  • the injection bores can be arranged in one or in both of the plates in order to open into the channel correspondingly on one or both sides.
  • the injection bores opening into the channel on both sides are preferably arranged offset relative to one another azimuthally. In this case, various dispersed phases can be alternately introduced side by side into the channel.
  • FIGS. 1 to 4 First, the geometry and in particular the mutual orientation of the supply line, the injection bores and the channel with the dispersion region in the emulsifying device according to the invention will be described. Details of the liquid transport into the supply line and the injection wells are exemplified in the FIGS. 5 to 10 shown.
  • the described emulsifying device is connected to a fluidic device for supplying liquid and controlling the emulsifying device. Details of the Fluidik worn (not shown), such as.
  • As liquid reservoirs, feed pumps, lines, valves and the like. Are known per se and are therefore not described here.
  • FIG. 1 shows the first embodiment of the emulsifying device 100 according to the invention with an inner part 110 and an outer part 120.
  • the inner part 110 has the shape of a straight circular cylinder with an outer diameter which is smaller than the inner diameter of the hollow cylindrical outer part 120.
  • the cylinder axes of the concentrically arranged inner and outer parts 110, 120 form the axial reference direction (z) of the emulsifying device 100.
  • the channel 20 (gap 20) is formed, which leads to the dispersion region 10.
  • the channel 20 is adapted for receiving a hollow cylindrical liquid layer of the continuous and dispersed phases 2, 3, which form liquid liquid filaments on liquid supply, which flow to the dispersion region 10.
  • the distance between the outer diameter of the inner part 110 and the inner diameter of the outer part 120 (radial channel height) is selected such that interfaces between the continuous and dispersed phases 2, 3 extend between the inner and outer parts 110, 120.
  • the radial channel height is selected, for example, in the range of 1 .mu.m to 0.1 mm.
  • the dispersion region 10 is formed by the mouth of the channel 20 into the surroundings of the emulsifying device 100.
  • the annular gap opening 11 is formed, at which the channel 20 extends stepwise in the radial direction.
  • the laminar liquid filaments of the continuous and dispersed phases 2, 3 in the channel 20 are unstable, so that they disintegrate into individual drops.
  • the droplet size is determined essentially by the radial channel height, which is the same for all droplets, so that advantageously a monodisperse droplet size distribution is generated.
  • the droplet size may be further influenced by a filling pressure or a delivery rate of the dispersed phases in the injection lines.
  • the filling pressure and / or the delivery rate of the dispersed phases may be in each injection line z. B. with a feed pump, in particular a syringe pump can be adjusted.
  • the feeding of the continuous phase 2 into the channel 20 takes place through the feed line 30.
  • the feed line 30, like the channel 20, is formed by the distance between the inner and outer parts 110, 120. Preferably, this distance in the regions of the channel 20 and the supply line 30, so that the channel 20 is substantially a continuation of the supply line 30.
  • the radial channel height in the channel 20 may deviate from the channel height in the supply line, in particular be smaller.
  • each injection well 42 extends from an injection port 43 in the outer surface of the outer member 120 to the channel 20.
  • an emulsion 1 comprising the continuous phase 2 and the dispersed phase 3
  • the continuous phase 2 is passed through the supply line 30 into the channel 20.
  • the feeding of the dispersed phase 3 through the injection bores 42 likewise takes place in the channel 20.
  • the flows of the continuous and dispersed phases 2, 3 flow as laminar liquid filaments to the dispersion region 10, at which the drop formation takes place.
  • the flow of the liquid filaments in the gap-shaped channel 20 is an essential feature for the production of monodisperse emulsions. Without the channel 20, the dispersed phase would expire on exiting small holes directly into the free environment even in single drops, but would have a polydisperse size distribution.
  • the droplets of the dispersed phase 3 flow in the variant according to FIG. 1 in the axial direction and with increasing distance from the gap opening 11 radially outwards, since the inner part 110 continues over the radial length of the outer part 120.
  • the outer part 120 can continue over the axial end of the inner part 110, as shown schematically in FIG FIG. 2 is illustrated.
  • the dispersion region 10 the channel 20, the supply line 30, and the injection wells 42 are as in FIG FIG. 1 arranged, which is limited by the limiting effect of the outer part 120, the exiting through the gap mouth 11 in the environment emulsion 1 radially inwardly.
  • FIGS. 3 and 4 show two variants of the second embodiment of the invention, in which the supply line 30 also extends in the axial direction of the emulsifying device 100, the channel 20, however, in contrast to the first embodiment ( FIGS. 1, 2 ) is aligned in the radial direction.
  • the upper and lower parts 130, 140 are arranged at a distance relative to each other, wherein between the mutually facing, flat side surfaces of the upper and lower parts 130, 140 of the channel 20 is formed.
  • the upper part 130 has the shape of a straight hollow cylinder.
  • the supply line 30 for supplying the continuous phase 2 into the channel 20 is provided inside the upper part 130.
  • the injection bores 42 also extend in the axial direction in the upper part 130. They extend parallel to the supply line 30 from the injection openings 43 to the channel 20. For reasons of clarity, only two injection bores 42 are illustrated again.
  • the continuous phase 2 is conducted through the supply line 30 into the channel 20.
  • the dispersed phase 3 is conducted from an injection line 40 above the upper part 130 via the injection bores 42 into the channel 20.
  • the continuous and the dispersed phase 2, 3 radially outwardly flowing laminar remplisstechniksfilrait formed at the annular gap mouth 11 of the dispersion region 10 decay into single drops according to the mechanism described above.
  • FIG. 4 shows a modified variant of the second embodiment of the emulsifying device 100 according to the invention, in which the supply line 30 is formed outside of the upper part 130 and the continuous and dispersed phases 2, 3 in the channel 20 to flow radially inwardly. Accordingly, the emulsion 1 is generated inside the hollow cylindrical shell 130.
  • the injection holes 40 of the emulsifying device 100 according to the Figures 1 or 2 can be applied alternately with different dispersed phases, so a mixed emulsion can be generated accordingly.
  • the structure of the emulsifying device 100 for producing the mixed emulsion can be simplified if the different dispersed phases 3 are injected into the channel 20 on both sides. Details of corresponding variants of the first embodiment of the emulsifying device according to the invention are in the FIGS. 5 and 6 illustrated.
  • the emulsifying device 100 has a concentric construction of the inner and outer parts 110, 120.
  • the outer part 120 comprises a hollow cylinder, in whose wall a first injection line 40 extends. From the first injection line 40, the first dispersed phase 3.1 can be injected into the channel 20 via external injection bores 42.
  • the inner part 110 likewise comprises a hollow cylinder in which a second injection line 41 extends, from which the second dispersed phase 3.2 can be injected into the channel 20 via inner injection bores 42.
  • the injection bores 42 each have funnel-shaped injection openings 43.
  • the channel 20 and the supply line 30 are formed by the distance between the inner and outer parts 110, 120, as described above.
  • the first embodiment of the invention has the advantage that the mixing emulsion 1 is produced at the front side of the emulsifying device 100 with a high density.
  • the continuous phase 2 and the dispersed phases 3.1, 3.2 are introduced into the channel 20.
  • laminar liquid filaments are formed, wherein the first and second dispersed phases are preferably arranged alternately side by side.
  • the dispersed phases decompose according to the mechanism described above into single drops distributed in the continuous phase.
  • the mixing ratio of the dispersed phases 3.1, 3.2 in the continuous phase 2 can be adjusted by the volume flows in the first and second injection lines 40, 41.
  • a droplet size ratio can also be set.
  • the droplets with defined droplet number densities form a specific arrangement in the structure of the emulsion.
  • FIG. 6 A further variant of the first embodiment of the emulsifying device 100 according to the invention is shown in FIG. 6 exemplified.
  • the emulsifying device 100 comprises the inner part 110 and the outer part 120, in which the injection lines 41, 40 are arranged.
  • the supply line 30 in the gap between the inner and outer parts 110, 120 is connected via a line connection (not shown) with a reservoir of the continuous phase.
  • the first and second injection lines 40, 41 are respectively connected to reservoirs of the first and second dispersed phases.
  • the injection holes are in the immediate vicinity of the dispersion area 10.
  • the axial length of the channel 20 from the injection holes to the gap mouth can be chosen so small that in the channel 20 just the stable laminar remplisstechniksfil noir be formed.
  • the axial length of the channel 20 may be selected, for example, in the range of 10 microns to 1 mm.
  • the emulsifying device 100 according to FIG. 5 or 6 is manufactured by providing the inner and outer parts 110, 120 by mechanical shaping (for example turning) and providing them with the injection bores 42 and the injection openings 43.
  • the holes can be generated for example by means of spark erosion.
  • available lithography techniques, etching processes, and / or electroplating techniques may be used.
  • the emulsifying device 100 according to FIG. 6 was tested in practice in which by the first injection line 40 and water through the second injection line 41 an oil-surfactant mixture (mono-olein in tetradecane) were led to the dispersion region 10. Within a few seconds, a volume of about one eighth of a cubic centimeter could be filled with a mixed emulsion of the two dispersed phases.
  • the radial channel height (distance between the inner and outer parts 110, 120) was 50 ⁇ m.
  • the diameter of the injection wells was around 100 ⁇ m.
  • the droplet size of the dispersed phases was around 200 ⁇ m. To produce smaller drop diameters, the injection wells can be provided with a correspondingly reduced diameter.
  • FIGS. 7 and 8 show further variants of the second embodiment of the emulsifying device 100 according to the invention for generating a radially outwardly, to a peripheral edge 12 of the emulsifying 100 flowing mixing emulsion (see FIG. 3 ).
  • FIG. 7 shows a schematic sectional view of the intended to produce the mixing emulsion 1 parts of the emulsifying 100.
  • the top and bottom parts 130, 140 include two round plates, the two planar, corresponding to the desired channel height z 0 spaced side surfaces.
  • FIG. 8 Illustrates the top view of the top 130.
  • the supply line 30 for supplying the continuous phase 2 is provided in the middle of the upper and lower parts 130, 140.
  • the injection bores 42 have funnel-shaped injection openings 43, which are connected via an annular groove 44.
  • Injection holes 42 are provided both in the upper part 130 and in the lower part 140. From the two sides of the channel 20, various dispersed phases 3.1, 3.2 are introduced into the channel.
  • the structure according to the FIGS. 7 and 8 can be realized, for example, with the following dimensions.
  • the upper and lower parts 130, 140 have a diameter of 2 cm.
  • the distance z 0 of the upper and lower parts 130, 140 and thus the axial channel height is preferably comparable to the diameter of the injection holes 42 or less than this, for example in the range of 1 .mu.m to 0.1 mm.
  • the number of injection bores 42 in the upper and lower parts 130, 140 is preferably the same size (for example, 240).
  • the hole circle formed by the injection holes 42 has a radius of about 8 mm.
  • the injection holes 42 are arranged at a distance which is preferably greater than twice the bore diameter, for example in the range of 5 microns to 0.5 mm, is selected and z. B. at a diameter of 30 microns is about 120 microns. Accordingly, 480 liquid filaments each with a width of about 30 microns can be formed. The width of the liquid filaments grows slightly in the radial direction, because the liquids flow slower due to the growing extent to the outside.
  • the upper and lower parts 130, 140 are arranged so rotated relative to each other that the injection holes 42 different azimuth angles relative to the radial reference direction of Emulsifier 100 have.
  • the various dispersed phases can advantageously be arranged side by side in the channel 20.
  • the continuous phase 2 and the dispersed phases 3.1, 3.2 are introduced into the channel 20. From each liquid entering into the channel 20 through one of the injection bores 42, a liquid filament is formed whose boundary surface is spanned relative to the liquid of the continuous phase 2 between the walls of the channel 20, ie between the upper and lower parts 130, 140. By acting on all of the injection bores 42 with dispersed phases, a ring of liquid filaments is formed in the gap-shaped channel 20 and flows radially and laminarly outwards in the flow of the continuous phase 2.
  • the differently dispersed phases 3.1, 3.2 are arranged azimuthally alternately next to each other. When the liquid filaments flow radially outward through the circular gap mouth 11 of the dispersion region 10, they decompose into single droplets in the free environment.
  • FIG. 9 shows a structure analogous to FIG. 7 with an upper part 130 and a lower part 140, between which the channel 20, the supply line 30 and the injection bores 42 are formed.
  • the continuous phase 2 is transported by the supply line 30 radially inward to the channel 20, where the injection of the dispersed phases 3.1, 3.2 takes place on both sides.
  • the radially inwardly flowing liquid filaments in the channel 20 decay at the gap mouth 11 of the dispersion region 10 into individual drops.
  • the emulsion 1 formed is transported away in the axial direction.
  • the upper and lower parts 130, 140 for providing the injection bores 40 and the corresponding injection lines 41, 42 are composed of a plurality of structured plates. Between the upper and lower parts 130, 140, an azimuthally interrupted spacer 21 is provided to form the channel 20, through which the continuous phase 2 and the dispersed phases 3.1, 3.2 flow to the channel 20.

Claims (27)

  1. Dispositif d'émulsification (100) destiné à former une émulsion (1) avec une phase continue (2) et au moins une phase dispersée (3, 3.1, 3.2), comprenant :
    - une zone de dispersion (10) destinée à former l'émulsion (1),
    - un canal (20) menant à la zone de dispersion (10) et prévu pour la réception de filaments liquides à flux laminaire des phases continue et dispersée(s) (2, 3, 3.1, 3.2),
    - une conduite d'alimentation (30) pour l'amenée de la phase continue (2) dans le canal (20), et
    - au moins une conduite d'injection (40, 41) pour l'amenée de la ou des phases dispersées (3, 3.1, 3.2) dans le canal (20),
    caractérisé
    - en ce qu'au moins une conduite d'injection (40, 41) est reliée au canal (20) par une pluralité d'orifices d'injection (42), et
    - en ce que la zone de dispersion (10) comprend un orifice en fente (11) du canal (20), lequel s'ouvre vers l'environnement du dispositif d'émulsification (100).
  2. Dispositif d'émulsification selon la revendication 1, où l'orifice en fente (11) a un tracé d'ouverture incurvé sur un plan, perpendiculairement à une direction de référence axiale (z) du dispositif d'émulsification (100).
  3. Dispositif d'émulsification selon la revendication 2, où l'orifice en fente (11) a un tracé d'ouverture représenté par une courbe géométriquement fermée.
  4. Dispositif d'émulsification selon la revendication 3, où l'orifice en fente (11) a un tracé d'ouverture circulaire.
  5. Dispositif d'émulsification selon l'une au moins des revendications précédentes, où deux conduites d'injection (40, 41) sont prévues, dont les orifices d'injection (42) débouchent respectivement sur deux côtés opposés du canal (20).
  6. Dispositif d'émulsification selon la revendication 5, où les orifices d'injection (42) de l'une des conduites d'injection (40) sont décalés par rapport aux orifices d'injection (42) de l'autre conduite d'injection (41).
  7. Dispositif d'émulsification selon l'une au moins des revendications précédentes, où les orifices d'injection (42) sont pourvus de cols d'injection en forme d'entonnoirs (43).
  8. Dispositif d'émulsification selon la revendication 7, où les cols d'injection en forme d'entonnoirs (43) sont reliés entre eux par une rainure (44).
  9. Dispositif d'émulsification selon l'une au moins des revendications précédentes, où le canal (20) s'étend parallèlement à la direction de référence axiale (z).
  10. Dispositif d'émulsification selon la revendication 9, où les orifices d'injection (40) s'étendent sur un plan, perpendiculairement à la direction de référence axiale (z).
  11. Dispositif d'émulsification selon la revendication 9 ou la revendication 10, où la ou les conduites d'injection (40, 41) et la conduite d'alimentation (30) sont disposées concentriquement entre elles.
  12. Dispositif d'émulsification selon la revendication 11, ayant la forme d'un cylindre, où la ou les conduites d'injection (40, 41) et la conduite d'alimentation (30) sont disposées concentriquement entre elles, l'orifice en fente (11) du canal (20) étant ménagé sur la face frontale du dit cylindre.
  13. Dispositif d'émulsification selon l'une au moins des revendications 1 à 10, où le canal (20) s'étend sur un plan, perpendiculairement à la direction de référence axiale (z).
  14. Dispositif d'émulsification selon la revendication 13, où le canal (20) s'étend radialement tout autour de la conduite d'alimentation (30) vers un bord périphérique (12) du dispositif d'émulsification.
  15. Dispositif d'émulsification selon l'une au moins des revendications 13 ou 14, où les orifices d'injection (42) s'étendent parallèlement à la direction de référence axiale (z) du dispositif d'émulsification.
  16. Dispositif d'émulsification selon l'une au moins des revendications 13 à 15, où le canal (20) est formé entre deux plateaux (130, 140), lesquels s'étendent perpendiculairement à la direction de référence axiale (z) du dispositif d'émulsification.
  17. Dispositif d'émulsification selon la revendication 16, où les orifices d'injection (42) sont prévus sur un des plateaux (130, 140) et débouchent unilatéralement dans le canal (20).
  18. Dispositif d'émulsification selon la revendication 16, où les orifices d'injection (42) sont prévus sur les deux plateaux (130, 140) et débouchent des deux côtés dans le canal (20).
  19. Dispositif d'émulsification selon la revendication 18, où les orifices d'injection (42) sont décalés entre eux sur les deux plateaux (130, 140).
  20. Procédé pour la formation d'une émulsion (1) avec une phase continue (2) et au moins une phase dispersée (3, 3.1, 3.2) au moyen d'un dispositif d'émulsification (100), comprenant les étapes suivantes :
    - amenée de la phase continue (2) dans un canal (20) au moyen d'une conduite d'alimentation (30),
    - amenée de la ou des phases dispersées (3, 3.1, 3.2) dans le canal (20) par au moins une conduite d'injection (40),
    - formation de filaments liquides à flux laminaire de la phase continue (2), et de la ou des phases dispersées (3, 3.1, 3.2), les filaments liquides s'écoulant les uns à côté des autres dans le canal (20) vers une zone de dispersion (10), et
    - formation de l'émulsion (1) à partir de la phase continue (2), et de la ou des phases dispersées (3, 3.1, 3.2) dans la zone de dispersion (10),
    caractérisé
    - en ce que pour l'amenée de la ou des phases dispersées (3, 3.1, 3.2), il est prévu une injection de la ou des phases dispersées (3, 3.1, 3.2) dans le canal (20) par une pluralité d'orifices d'injection (42), et
    - en ce que la formation de l'émulsion (1) comprend une sortie de la phase continue (2) et de la ou des phases dispersées (3, 3.1, 3.2) vers l'environnement du dispositif d'émulsification, par l'orifice en fente (11) du canal (20).
  21. Procédé selon la revendication 20, où la ou les phases dispersées (3, 3.1, 3.2) sont amenées sur deux côtés opposés du canal (20) par des orifices d'injection (42).
  22. Procédé selon la revendication 21, où la ou les phases dispersées (3, 3.1, 3.2) sont amenées par deux conduites d'injection séparées (40, 41) vers les orifices d'injection (42) des deux côtés du canal (20).
  23. Procédé selon l'une au moins des revendications 20 à 22, où la sortie de la phase continue (2), et de la ou des phases dispersées (3, 3.1, 3.2) par l'orifice en fente (11) du canal (20), est prévue dans une direction parallèle à la direction de référence axiale (z).
  24. Procédé selon l'une au moins des revendications 21 à 22, où la sortie de la phase continue (2), et de la ou des phases dispersées (3, 3.1, 3.2) par l'orifice en fente (11) du canal (20), est prévue sur un plan, perpendiculairement à la direction de référence axiale (z).
  25. Procédé selon l'une au moins des revendications 21 à 24, où il est prévu une amenée de deux phases dispersées (3, 3.1, 3.2) dans le canal (20), et où un mélange des phases dispersées (3, 3.1, 3.2) est effectué à la sortie de la phase continue (2) et des phases dispersées (3, 3.1, 3.2) par l'orifice en fente (11) du canal (20).
  26. Procédé selon la revendication 25, comprenant l'étape suivante :
    - définition d'un rapport de mélange prescrit pour les phases dispersées (3, 3.1, 3.2).
  27. Procédé selon la revendication 26, où la définition du rapport de mélange prescrit pour les phases dispersées (3, 3.1, 3.2) comprend une définition de la viscosité des phases dispersées, d'une pression de remplissage et/ou d'un débit de refoulement des phases dispersées.
EP07786556A 2006-08-07 2007-08-03 Dispositif d'émulsification et procédé de formation d'une émulsion Not-in-force EP2049235B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006036815A DE102006036815B4 (de) 2006-08-07 2006-08-07 Emulgiereinrichtung und Verfahren zur Bildung einer Emulsion
PCT/EP2007/006899 WO2008017429A1 (fr) 2006-08-07 2007-08-03 Dispositif d'émulsification et procédé de formation d'une émulsion

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EP2049235A1 EP2049235A1 (fr) 2009-04-22
EP2049235B1 true EP2049235B1 (fr) 2010-06-09

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WO (1) WO2008017429A1 (fr)

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JP6912161B2 (ja) * 2016-02-25 2021-07-28 株式会社神戸製鋼所 流路装置及び液滴形成方法

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US7485671B2 (en) * 2003-05-16 2009-02-03 Velocys, Inc. Process for forming an emulsion using microchannel process technology
EP1804964A1 (fr) * 2004-10-01 2007-07-11 Velocys Inc. Procede de melange multiphase par technologie de traitement a micro-canaux
DE102005037401B4 (de) * 2005-08-08 2007-09-27 MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. Bildung einer Emulsion in einem fluidischen Mikrosystem

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DE102006036815B4 (de) 2010-01-14
ATE470497T1 (de) 2010-06-15
WO2008017429A1 (fr) 2008-02-14
US20090312442A1 (en) 2009-12-17
DE502007004085D1 (de) 2010-07-22
DE102006036815A1 (de) 2008-02-28
EP2049235A1 (fr) 2009-04-22

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