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WO2003068381A1 - Procede pour la production de nanogouttes monodispersees et dispositif pour l'execution de ce procede - Google Patents

Procede pour la production de nanogouttes monodispersees et dispositif pour l'execution de ce procede Download PDF

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Publication number
WO2003068381A1
WO2003068381A1 PCT/EP2003/001418 EP0301418W WO03068381A1 WO 2003068381 A1 WO2003068381 A1 WO 2003068381A1 EP 0301418 W EP0301418 W EP 0301418W WO 03068381 A1 WO03068381 A1 WO 03068381A1
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WIPO (PCT)
Prior art keywords
fluid
module
microfluidic reactor
focusing module
fluids
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PCT/EP2003/001418
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German (de)
English (en)
Inventor
Steffen Hardt
Volker Hessel
Original Assignee
INSTITUT FüR MIKROTECHNIK MAINZ GMBH
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Publication of WO2003068381A1 publication Critical patent/WO2003068381A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • 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
    • 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
    • B01F23/414—Emulsifying characterised by the internal structure of the emulsion
    • B01F23/4143—Microemulsions
    • 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
    • B01F25/3132—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit by using two or more injector devices
    • 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
    • B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
    • 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
    • B01F33/05—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material
    • 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
    • B01F33/05—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material
    • B01F33/052—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material the energy being electric fields for electrostatically charging of the ingredients or compositions for mixing them
    • 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
    • B01F33/05—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material
    • B01F33/053—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material the energy being magnetic or electromagnetic energy, radiation working on the ingredients or compositions for or during mixing them
    • 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
    • B01F33/05—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material
    • B01F33/054—Mixers using radiation, e.g. magnetic fields or microwaves to mix the material the energy being in the form of a laser to modify the characteristics or conditions of the products, e.g. for heating
    • 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
    • B01F33/3011—Micromixers using specific means for arranging the streams to be mixed, e.g. channel geometries or dispositions using a sheathing stream of a fluid surrounding a central stream of a different fluid, e.g. for reducing the cross-section of the central stream or to produce droplets from the central stream
    • 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
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/94—Heating or cooling systems using radiation, e.g. microwaves or electromagnetic radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying

Definitions

  • the invention relates to a method for producing monodisperse nanodroplets and to a microfluidic reactor for carrying out the method.
  • a method and a device for producing nanoparticles is described in the publication "Aero-sol-gel Reactor for nano-powder-synthesis" by G. Beaucage et al., Journal of Nanoparticle Research 1 (1999) 379-392.
  • the nanoparticles are generated by sol-gel reactions in aerosols.
  • the Aero-Sol-Gel reactor allows the structure, chemical composition and outer surface of silicon oxide powders to be influenced by changing the process parameters.
  • the Aero-Sol-Gel reactor contains a dry nitrogen, which is bubbled through precursor liquids to form steam flows.
  • the blowing device can be heated to control the concentrations of the reactants in the feed streams.
  • TEOS tetraethoxysilane
  • three steam flows are given up in a laminar flow, namely TEOS, water and hydrochloric acid. All process steam flows are heated to approx. 110 ° C to prevent premature condensation.
  • the laminar flows flow into an air mix / condensation / reaction zone, which is similar to that of pyrolytic reactors.
  • the nano-structured powders are then collected in a funnel-shaped filter.
  • the main disadvantage of the known methods is the poor controllability of the particle size and shape.
  • the size and size distribution of the particles largely depends on the reaction conditions, such as temperature, pressure and concentrations, which as a rule cannot be set arbitrarily. The same applies to the shape of the particles.
  • the object of the invention was to develop a method with which nanotropic droplets or nanoparticles of spherical geometry and a defined size can be produced.
  • Another subtask consists in providing a microfluidic reactor for performing the method.
  • the object is achieved with a method in which an immiscible second fluid B is introduced into a continuously flowing first fluid A, in which the fluid B is surrounded by the fluid A and in which the flow cross section of the fluid B is tapered in the direction of flow, that the fluid B disintegrates into individual drops due to its hydrodynamic instability.
  • the main advantage of this method is the ability to change the size of the fluid simply by selecting the fluid flow rates without having to make any changes to a device to be able to control the resulting particles.
  • the optimally desired spherical shape of the particles with a predeterminable particle size is achieved.
  • the fluids A, B are advantageously accelerated in a focusing module by a geometric cross-sectional reduction and fed to a drop formation channel with a constant opening width.
  • the geometric cross-sectional reduction in the focusing module is an easy-to-implement option for tapering the flow cross-section of the fluids in the direction of flow.
  • the geometric cross-sectional reduction can be achieved using a decreasing cross-section, e.g. a funnel or via a step-like reduction in the opening width. In the case of a step-like reduction in the opening width, stationary vortices can form in the storage space of the steps, but these have no influence on the principle of action.
  • a fluid A is supplied to a fluid stream B via inlet openings distributed in the flow direction. This significantly reduces the risk of blockages due to particles already forming in the drop formation channel.
  • the fluid A After flowing through the focusing module, the fluid A is preferably returned in a return flow channel against the flow direction. As a result, the fluid A can be reused and its consumption can be minimized.
  • a control fluid X is advantageously introduced into the fluid A via an access.
  • the location of the drop formation in the drop formation channel can be influenced, since the location of the drop formation depends not only on the size of the flow cross section, but also on material parameters such as density, viscosity and surface tension.
  • the fluids A, B are advantageously fed to the focusing module via a distributor module.
  • the distributor module is used to apply the fluids A, B with defined initial conditions.
  • a plurality of parallel-spaced fluid streams B are emitted from the distributor module into the focusing module.
  • the flow rate and thus the conversion can be increased and the pressure drop reduced.
  • the drop formation channel has a very small flow cross section.
  • several fluid flows B allow a larger flow cross section.
  • a force is advantageously exerted on electrically conductive fluids A, B by means of a magnetic coil or a solid-state magnet.
  • the electrically conductive fluids A, B flow through a magnetic field in which they are stabilized. With the help of the magnetic field, for example, premature decay into drops could be prevented.
  • Both magnetic coils and solid-state magnets can be used to generate the magnetic field.
  • the fluids A, B are advantageously irradiated with a laser. Fluid B could be heated with the help of the laser, which in turn changes the properties of the material. In this way, the location of the drop formation in the drop formation channel can be influenced.
  • the method can also be carried out advantageously by supplying the focusing module with a third fluid C, the fluid B being chosen to be hydrodynamically unstable than the fluid C. Fluid B and fluid B should be surrounded by fluid A in the direction of flow of the fluid C, ie the fluid streams should be nested within one another. This type of fluid application, in conjunction with the requirement that the fluid B is more hydrodynamically unstable than the fluid C, enables concentric drops of the fluid C in the fluid B. The fluid C is completely surrounded by the fluid B.
  • Another alternative can also be useful, in which the fluid C is chosen to be more unstable than the fluid B. This can then be used to generate drops of fluid B which contain a number of smaller drops C.
  • a voltage can advantageously be impressed into the fluids A, B, at least one fluid A or fluid B having electrolytic properties.
  • a defined electrical charge can be applied to the fluid A or fluid B, as a result of which drop agglomerations and drop coalescence are prevented.
  • the outer fluid A and the inner fluid B can be in contact with an anode and a cathode, one of which is located in the region of the distributor module and the other in the region of the reaction module. If Fluid B has electrolytic properties and there is an electrode at the reactor inlet, charges in Fluid B migrate away from the electrode to the location of the drop formation. As a result, a defined charge is applied to the drops, which prevents the drops from coalescing and makes it possible to collect the drops or the particles formed from the drops on the counterelectrode.
  • Nanoparticles which are produced by the processes known from the prior art do not achieve such a narrow particle size distribution and particle shape.
  • the size of the nanoparticles can be controlled very precisely with the method according to the invention through the choice of the geometric cross-sectional reduction or the setting of the hydrodynamic conditions and the choice of the quantitative ratios of the fluids.
  • Nanoparticles produced by the method according to the invention are of great importance for many relatively new fields of application, such as coatings for surfaces, catalysts, etc.
  • the particles are preferably generated in the reaction module by polymerization. This permits spatial separation of the process steps, formation of the drops in the drop formation channel and formation of the particles in the subsequent reaction module.
  • a solution of monomers is advantageously used as fluid B.
  • monomers are in the form of a fluid.
  • the polymerization is preferably induced by adding initiators. With the addition of initiators, the location and time of particle formation can be controlled.
  • the polymerization is favorably induced by introducing heat or light. Both possibilities represent simple methods to initiate the polymerization and thus the formation of the particles.
  • the subtask is solved with a microfluidic reactor in which a second fluid stream of a fluid B is introduced in a first continuous fluid stream of a fluid A, the fluid B being surrounded by fluid A and the fluids A, B being immiscible and in the one Focusing module is formed with an inlet funnel tapering in the direction of flow, to which a drop formation channel is connected at its small opening end.
  • the device constructed in this way enables a defined generation of nanotropes or nanoparticles with a spherical geometry and a defined size.
  • the microfluidic reactor does not require small, difficult-to-manufacture microstructures for shaping the fluid streams, which can be chosen to be larger than the nanotropes or nanoparticles, which in particular reduces the manufacturing outlay.
  • the focusing module does not necessarily have to have an inlet funnel that continuously narrows in the narrower sense. The tapering of the fluid cross-sections can also be achieved by step-like cross-sectional constrictions in the focusing module.
  • a distributor module for supplying the fluids A, B into the focusing module is formed with a plurality of outlet channels of the fluid A and outlet channels of the fluid B.
  • the outlet channels of the fluid B preferably have an opening width of 100 nm to 500 ⁇ m, an opening width of 1 ⁇ m to 100 ⁇ m having been found to be particularly advantageous.
  • the drop formation channel has the opening width of the small opening end of the inlet channel.
  • a second fluid stream of a fluid B is introduced in a first continuous fluid stream of a fluid A, the fluid B being completely surrounded by the fluid A and the fluids A, B being immiscible and in a focusing module a substantially constant opening width, in which inlet openings for supplying the fluid A are arranged offset in the flow direction in at least one peripheral wall of the focusing module, and in which a drop formation channel is connected to the focusing module.
  • Such a microfluidic reactor focuses the fluid flows hydrodynamically.
  • the microfluidic reactors can be provided with larger structures that are easier to manufacture, since the cross section of the second fluid flow is not tapered by the geometry of the microfluidic reactor, but by a repeated metering in of the fluid A.
  • the focusing module of the microfluidic reactor described above preferably has separating structures for delimiting a backflow channel.
  • the separation structures enable better guidance of the fluid A.
  • a reaction module is advantageously connected to the drop formation channel in the flow direction.
  • the reaction module has inlet openings through which, for example, initiators for initiating a polymerization can be added. This allows the location and time of particle formation to be controlled.
  • the reaction module preferably comprises a heat or light source in order to initiate the polymerization reaction and thus the formation of the particles.
  • a magnet coil is advantageously arranged on the focusing module.
  • a magnetic field is built up via the magnetic coil, which stabilizes the electrically conductive fluids and prevents premature decay in the drop.
  • a solid-state magnet can also be used instead of the magnetic coil.
  • a laser is advantageously arranged on the drop formation channel.
  • the two fluids A, B can be heated by means of the laser, as a result of which the material properties change. In this way, the location of the drop formation can be influenced.
  • an electrode is attached to each of the distributor module and the reaction module, with which a voltage can be impressed into the fluids A, B.
  • Figure 1 is a schematic representation of a microfluidic reactor according to a first embodiment
  • FIG. 2 shows a schematic illustration of a microfluidic reactor according to a first embodiment with a plurality of parallel flows of the fluid B;
  • FIG. 3 shows a microfluidic reactor according to FIG. 2 with a magnetic coil arranged outside the reactor;
  • FIG. 4 shows a microfluidic reactor according to FIG. 2 with a laser;
  • Figure 5 is a schematic representation of a microfluidic reactor according to the first embodiment for encapsulating a third fluid C;
  • FIG. 6 shows a microfluidic reactor according to FIG. 1 with electrodes on the distributor module and reaction module;
  • FIG. 7 shows a schematic illustration of a microfluidic reactor according to a second embodiment
  • FIG. 8 shows a microfluidic reactor according to FIG. 7 with two opposite return flow channels
  • Figure 9 is a schematic representation of a microfluidic reactor with inlet openings for the control fluid X.
  • FIG. 1 schematically shows a microfluidic reactor according to a first embodiment, in which the flow of the fluids A, B is focused by the geometric configuration of the reactor.
  • the fluids A, B flow in the flow direction 2 through a cross-sectional reduction 27 into the drop formation channel 5.
  • the Outlet channel 8 of the fluid B has an opening width 9 in the region of the transition into the focusing module 1, the dimension of which is typically a few micrometers. Due to the arrangement of the outlet channels 7 on both sides of the outlet channel 8, the fluid B is surrounded on both sides by the fluid A.
  • the geometric cross-sectional widening 27 Due to the geometric cross-sectional widening 27 from the opening width 11 of the focusing module 1 to the opening width 10 of the drop formation channel 5, there is a narrowed flow cross-section 16 of the fluid B.
  • the geometric cross-sectional widening 27 can take place in one or in two spatial directions.
  • the funnel walls 30 are shown perpendicular to the drop formation channel 5, so that a vortex or dead water zone 29 is formed.
  • the inclination of the funnel walls 30 with the end 31 on the peripheral wall side in the direction of the distributor module 6 can reduce or avoid the formation of the vortex and dead water zone 29.
  • a reaction module 17 is connected to the drop formation channel 5 in order to generate particles 28 from drops 26.
  • the actual particle formation takes place, for example, by polymerization under the influence of heat.
  • the heat is generated via a heat source 19 arranged outside the peripheral wall 32 of the reactor module 17.
  • FIG. 2 also shows a microfluidic reactor according to the first embodiment, that is to say with a geometrical focusing, but a plurality of parallel flows of the fluid A and the fluid B are alternately fed into the distributor module 6. As a result, the throughput of the fluids and thus the output on the droplet 26 or particles 28 (not shown) is increased.
  • the funnel walls 30 run toward one another in an arc shape in the direction of the small opening end 4 of the inlet funnel 3.
  • a reaction module 17 could follow the drop formation channel 5 to form particles 28 from the drops 26, but this is not shown in FIG. 2.
  • FIG. 3 shows an embodiment of the microfluidic reactor according to FIG. 2 with a magnet coil 21 which is arranged in the region of the peripheral wall 12 and is suitable for forming an axial magnetic field 24.
  • a force is exerted on the fluid B if its electrical conductivity is different from zero.
  • a finite conductivity could be achieved with the help of an electrolyte. It is known from magnetohydrodynamics that a sufficiently strong magnetic field can prevent a breakdown of fluid flows. It is thus possible to stabilize the flows of the fluid B in the focus module 1 and to limit the effect of the hydrodynamic instability and thus the formation of drops 26 on the drop formation channel 5.
  • FIG. 4 also shows a first embodiment of the microfluidic reactor, in which, however, a laser 22 is arranged in the area of the drop formation channel 5.
  • the pulsed laser embosses a periodic temperature profile on the streams of fluid B flowing through the drop formation channel 5.
  • the wavelength of the temperature profile makes it possible to determine the decay wavelength.
  • the size of the drops 26 can thus be influenced and variations beyond the ratio of drop size to size of the fluid flow of the fluid B which is characteristic of the undisturbed dynamics are possible.
  • selective influencing of specific fluids can be achieved by tuning the laser wavelength to the absorption bands of the molecules of the fluid B.
  • the distributor module 6 has an additional possibility of nesting a third fluid C in the fluid B, and in turn enclosing it surrounded by the fluid A.
  • a microfluidic reactor offers the possibility of producing drops 26 or particles 28 (not shown) made up of several layers. For this it is necessary to choose the material properties so that the formation of drops 26 of the fluid B takes place before the decay of the fluid flow of fluid C. In this case, the drops 26 or particles 28 (not shown) have a core 33 around a shell 34 made of different materials.
  • FIG. 6 shows a microfluidic reactor according to the first embodiment, to whose distributor module 6 cathodes 23a and in the area of the reaction module 17 an anode 23b are attached.
  • the field lines 36 are drawn as broken lines from the cathodes 23a to the anode 23b.
  • negative charges migrate in the fluid B having electrolytic properties from the cathode 23a to the location of the drops 26 in the drop formation channel 5. This brings a defined negative charge onto the drops, which prevents the drops 26 from coalescing and entering Collecting the drops 26 or the particles 28 at the anode 23b is possible.
  • a light source 20 is present in the area of the reaction module 17 to form the particles 28 by means of polymerization.
  • FIG. 7 shows a schematic illustration of a microfluidic reactor according to a second embodiment.
  • the fluid B is located in the center of the focusing module 1 or the droplet formation channel 5, surrounded by the fluid A.
  • the peripheral wall 12 of the focusing module 1 is provided with inlet openings 13, which successively supply the fluid A into the focusing module 1 allow.
  • the opening width 11 of the focusing module 1 is identical to the opening width 10 of the droplet formation channel 5.
  • the flow cross-section 25 of the fluid B is reduced without a geometric change in the microfluidic reactor solely from the supply of the fluid A.
  • FIG. 8 shows a preferred embodiment of the reactor according to FIG. 7, in which a partial flow reversal 37 of the fluid A takes place in the transition area 38 from the focusing module 1 to the drop formation channel 5, part of the fluid A in the return flow channel 15 separated by separating structures 14 flows back and flows again through the inlet openings 13 into the focusing module 1.
  • Figure 9 illustrates the second embodiment of the microfluidic reactor in which in the flow direction 2, an 'access 35 is formed for the addition of a control fluid X both sides behind the inlet ports 13 of the fluid A in the peripheral wall 12 of the focusing module. 1
  • the control fluid X enables the position of the formation of the drops 26 in the drop formation channel 5 to be influenced.
  • reaction module 9 heat source 0 light source 1 magnetic coil 2 laser 3a cathode 3b anode 4 magnetic field Flow cross-section, fluid B, second embodiment drop cross-section reduction particles vortex zone or dead water zone funnel wall circumferential end, funnel wall circumferential wall, reaction module core-shell access, control fluid X field lines, electric field flow reversal transition area, focusing module / drop formation channel

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  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
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  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne un procédé et un dispositif servant à produire des nanogouttes monodispersées. L'invention vise à obtenir une répartition de taille mieux contrôlable et une forme plus régulière des nanogouttes qu'avec les procédés et les dispositifs déjà connus. Le procédé selon l'invention pour la production de nanogouttes monodispersées est caractérisé en ce qu'on introduit dans un fluide A s'écoulant en continu un deuxième fluide B non miscible, en ce que le fluide B est entouré par le fluide A et en ce que la section d'écoulement (16, 25) du fluide B rétrécit dans le sens d'écoulement (2) de sorte que le fluide B se désagrège en gouttes individuelles (26) en raison de son instabilité hydrodynamique. L'invention concerne également un réacteur microfluidique pour l'exécution de ce procédé, dans lequel on introduit dans un premier flux continu d'un fluide A un deuxième flux d'un fluide B, le fluide B étant entouré par le fluide A et les fluides A et B n'étant pas miscibles. Le réacteur selon l'invention est caractérisé par un module de focalisation (1) comprenant une trémie d'entrée (3) rétrécissant dans le sens d'écoulement (2) et à l'extrémité (4) à petite ouverture de laquelle est raccordé un conduit de formation de gouttes (5).
PCT/EP2003/001418 2002-02-13 2003-02-13 Procede pour la production de nanogouttes monodispersees et dispositif pour l'execution de ce procede WO2003068381A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10206083A DE10206083B4 (de) 2002-02-13 2002-02-13 Verfahren zum Erzeugen monodisperser Nanotropfen sowie mikrofluidischer Reaktor zum Durchführen des Verfahrens
DE10206083.5 2002-02-13

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EP1415708A3 (fr) * 2002-11-01 2004-12-29 Hitachi, Ltd. Reacteur chimique et dispositif
WO2006051153A2 (fr) * 2004-11-09 2006-05-18 Nanolab Systems Oy Procedes et dispositifs pour simplifier la production de nanoparticules, et leurs applications
US7307104B2 (en) 2003-05-16 2007-12-11 Velocys, Inc. Process for forming an emulsion using microchannel process technology
US7485671B2 (en) 2003-05-16 2009-02-03 Velocys, Inc. Process for forming an emulsion using microchannel process technology
US7556776B2 (en) 2005-09-08 2009-07-07 President And Fellows Of Harvard College Microfluidic manipulation of fluids and reactions
US7622509B2 (en) 2004-10-01 2009-11-24 Velocys, Inc. Multiphase mixing process using microchannel process technology
EP1913994A3 (fr) * 2006-10-20 2009-12-02 Hitachi Plant Technologies, Ltd. Appareil d'émulsion et appareil de fabrication de grains fins
US7943671B2 (en) 2005-08-08 2011-05-17 Max-Planck-Gesellschaft Zur Foerderung Der Wissenschaften E.V. Formation of an emulsion in a fluid microsystem
US9573099B2 (en) 2011-05-23 2017-02-21 President And Fellows Of Harvard College Control of emulsions, including multiple emulsions
US9664619B2 (en) 2008-04-28 2017-05-30 President And Fellows Of Harvard College Microfluidic device for storage and well-defined arrangement of droplets
US10195571B2 (en) 2011-07-06 2019-02-05 President And Fellows Of Harvard College Multiple emulsions and techniques for the formation of multiple emulsions
US10316873B2 (en) 2005-03-04 2019-06-11 President And Fellows Of Harvard College Method and apparatus for forming multiple emulsions
WO2020074721A1 (fr) 2018-10-11 2020-04-16 Emulco Laboratories C.V.B.A. Procédé pour produire des émulsions et émulsion de polyisobutène aqueuse
US10874997B2 (en) 2009-09-02 2020-12-29 President And Fellows Of Harvard College Multiple emulsions created using jetting and other techniques

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JP4661942B2 (ja) * 2008-05-13 2011-03-30 ソニー株式会社 マイクロチップとその流路構造
US9782733B2 (en) 2012-03-22 2017-10-10 Universiteit Twente Apparatus and method for mass producing a monodisperse microbubble agent
DE102012010959B4 (de) * 2012-05-30 2019-03-28 Technische Universität Dresden Vorrichtung zur Bereitstellungkonstanter Strömungsverhältnisse vonunterschiedlichen Fluidphasen in Mikrokanalelementen
DE102017105194A1 (de) 2017-03-10 2018-09-13 Little Things Factory Gmbh Fokussiereinrichtung, Tropfengenerator und Verfahren zum Erzeugen einer Vielzahl von Tröpfchen

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US3329745A (en) * 1965-10-05 1967-07-04 Grange Lee D La Process for making gelled spherical particles of oxides
US3933679A (en) * 1972-01-14 1976-01-20 Gulf Oil Corporation Uniform microspheroidal particle generating method
US3962383A (en) * 1972-10-03 1976-06-08 Yoshiro Hagiwara Method and apparatus for manufacturing seamless material-filled capsules
CH563807A5 (en) * 1973-02-14 1975-07-15 Battelle Memorial Institute Fine granules and microcapsules mfrd. from liquid droplets - partic. of high viscosity requiring forced sepn. of droplets
US4251195A (en) * 1975-12-26 1981-02-17 Morishita Jinta Company, Limited Apparatus for making miniature capsules
US4422985A (en) * 1982-09-24 1983-12-27 Morishita Jintan Co., Ltd. Method and apparatus for encapsulation of a liquid or meltable solid material
WO1996011053A1 (fr) * 1994-10-07 1996-04-18 Warner-Lambert Company Procede de fabrication de capsules sans soudure
WO2000062913A1 (fr) * 1999-04-16 2000-10-26 INSTITUT FüR MIKROTECHNIK MAINZ GMBH Procede et micromelangeur pour la realisation d'une dispersion

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US7374726B2 (en) 2002-11-01 2008-05-20 Hitachi, Ltd. Chemical reactor
EP1415708A3 (fr) * 2002-11-01 2004-12-29 Hitachi, Ltd. Reacteur chimique et dispositif
US7307104B2 (en) 2003-05-16 2007-12-11 Velocys, Inc. Process for forming an emulsion using microchannel process technology
US7485671B2 (en) 2003-05-16 2009-02-03 Velocys, Inc. Process for forming an emulsion using microchannel process technology
US7816411B2 (en) 2004-10-01 2010-10-19 Velocys, Inc. Multiphase mixing process using microchannel process technology
US7622509B2 (en) 2004-10-01 2009-11-24 Velocys, Inc. Multiphase mixing process using microchannel process technology
WO2006051153A2 (fr) * 2004-11-09 2006-05-18 Nanolab Systems Oy Procedes et dispositifs pour simplifier la production de nanoparticules, et leurs applications
WO2006051153A3 (fr) * 2004-11-09 2006-06-29 Nanolab Systems Oy Procedes et dispositifs pour simplifier la production de nanoparticules, et leurs applications
US10316873B2 (en) 2005-03-04 2019-06-11 President And Fellows Of Harvard College Method and apparatus for forming multiple emulsions
US7943671B2 (en) 2005-08-08 2011-05-17 Max-Planck-Gesellschaft Zur Foerderung Der Wissenschaften E.V. Formation of an emulsion in a fluid microsystem
US7556776B2 (en) 2005-09-08 2009-07-07 President And Fellows Of Harvard College Microfluidic manipulation of fluids and reactions
EP1913994A3 (fr) * 2006-10-20 2009-12-02 Hitachi Plant Technologies, Ltd. Appareil d'émulsion et appareil de fabrication de grains fins
US9664619B2 (en) 2008-04-28 2017-05-30 President And Fellows Of Harvard College Microfluidic device for storage and well-defined arrangement of droplets
US10828641B2 (en) 2008-04-28 2020-11-10 President And Fellows Of Harvard College Microfluidic device for storage and well-defined arrangement of droplets
US11498072B2 (en) 2008-04-28 2022-11-15 President And Fellows Of Harvard College Microfluidic device for storage and well-defined arrangement of droplets
US10874997B2 (en) 2009-09-02 2020-12-29 President And Fellows Of Harvard College Multiple emulsions created using jetting and other techniques
US9573099B2 (en) 2011-05-23 2017-02-21 President And Fellows Of Harvard College Control of emulsions, including multiple emulsions
US10195571B2 (en) 2011-07-06 2019-02-05 President And Fellows Of Harvard College Multiple emulsions and techniques for the formation of multiple emulsions
WO2020074721A1 (fr) 2018-10-11 2020-04-16 Emulco Laboratories C.V.B.A. Procédé pour produire des émulsions et émulsion de polyisobutène aqueuse
EP3646941A2 (fr) 2018-10-11 2020-05-06 Emulco Laboratories C.V.B.A. Procédé de production d'émulsions et émulsion aqueuse de polyisobutène

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