WO2013014216A1 - Dispositif et procédé pour la production et la fusion à haut débit à la demande de gouttelettes - Google Patents

Dispositif et procédé pour la production et la fusion à haut débit à la demande de gouttelettes Download PDF

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Publication number
WO2013014216A1
WO2013014216A1 PCT/EP2012/064641 EP2012064641W WO2013014216A1 WO 2013014216 A1 WO2013014216 A1 WO 2013014216A1 EP 2012064641 W EP2012064641 W EP 2012064641W WO 2013014216 A1 WO2013014216 A1 WO 2013014216A1
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Prior art keywords
pressure buffer
fluid
fhe
microchannels
droplets
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Application number
PCT/EP2012/064641
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English (en)
Inventor
Jan GUZOWSKI
Piotr Korczyk
Sławomir JAKIEŁA
Piotr Garstecki
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Instytut Chemii Fizycznej Polskiej Akademii Nauk
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Publication of WO2013014216A1 publication Critical patent/WO2013014216A1/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
    • 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
    • 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
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
    • B01F33/813—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles mixing simultaneously in two or more mixing receptacles
    • 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
    • B01F35/20—Measuring; Control or regulation
    • B01F35/21—Measuring
    • B01F35/211—Measuring of the operational parameters
    • 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
    • B01F35/20—Measuring; Control or regulation
    • B01F35/22—Control or regulation
    • B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
    • B01F35/2211—Amount of delivered fluid during a period
    • 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
    • B01F35/71—Feed mechanisms
    • B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
    • B01F35/71755—Feed mechanisms characterised by the means for feeding the components to the mixer using means for feeding components in a pulsating or intermittent manner
    • 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
    • B01F35/71—Feed mechanisms
    • B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
    • B01F35/71805—Feed mechanisms characterised by the means for feeding the components to the mixer using valves, gates, orifices or openings

Definitions

  • the invention relates to a device and a method for high throughput, on demand generation of droplets.
  • the invention finds application in microfluidics and in performing chemical reactions in microvolumes.
  • emulsions Suspensions of microscopic droplets resulting from dispersing one liquid phase in another liquid phase - called emulsions - apart from being common in natu re ( biologic a l su bsta nces) a re used a lso in a n u m ber of ind ustria l applications including manufacturing of paints, cosmetics and drugs.
  • Most cosmetic creams and lotions are emulsions, and their properties are direct functions of the degree of dispersion, droplet stability, and size distribution. Emulsions are also often used in drug manufacturing because of better delivery and absorption of active ingredients.
  • emulsions are manufactured in industrial scale with the use of emulsifiers, i.e. surface active agents that facilitate generation and increase stability of droplets by reducing surface tension between selected fluids.
  • emulsifiers i.e. surface active agents that facilitate generation and increase stability of droplets by reducing surface tension between selected fluids.
  • the dispersing is usually accomplished by intensive and vigorous mixing of two liquid components.
  • aerosols suspensions of liquid droplets in gas, e.g., in air
  • the method allows for a high-throughput generation of emulsions, but the dispersion of droplet size exceeds 10%.
  • new applications in chemical microanalysis, biotechnology and microencapsulation of pharmaceuticals have created high demand for capabilities to produce droplets with precisely defined sizes.
  • a high degree of control over the droplet volume is offered by microfluidic devices producing droplets with geometries of typical sizes of a few to a few hu ndreds micrometers. Many solutions have been reported. Joscelyne and Tragardh (Journal of Membrane Science, 2000,
  • Droplet formulation in microchannels is a spontaneous process that takes place when flows of two immiscible fluids are crossed with each other.
  • the droplet generation mechanism depends essentially on the geometry of the junction.
  • the most often used solutions are flow-focusing junctions [P. Garstecki ef al. Physical Review Letters, 2005, 94, 104501 ], or T-junctions [P. Guillot, A. Colin, Physical Review E, 2005, 72, 066301].
  • the droplet phase is supplied from one channel, whereas the continuous phase is supplied from two channels focused at the spot where the droplets are produced.
  • the droplet phase is swept away by a perpendicular flow of the continuous phase.
  • An attempt to solve the low throughput problem may be to multiply the flow into many parallel channels supplied from a single source [T. Nisisako, T. Torii, Lab on a Chip, 2008, 8, 287-293].
  • the solution does not eliminate, however, the remaining limitations related to the spontaneous droplet generation, and simply increases them as branches may adversely affect the monodispersity of droplets as a result of uneven flow distribution in individual channels [V. Barbier ef a/., Physical Review E, 2000, 74, 04030 ⁇ ; W. Li ef a/., Soft Matter 2008, 4, 258].
  • An additional hindrance are fluctuations of the system supply pressure that are difficult to eliminate and translate into fluctuations of the flow rate of each phase, and therefore of the sizes of droplets produced in the system.
  • the device for high-throughput, on-demand generation of droplets is characterised in that it comprises n>2 microchannels originating at the first pressure buffer and n corresponding microchannels, originating at the second pressure buffer, whereas the said microchannels meet in pairs in n microfluidic junctions.
  • the said first pressure buffer is connected to the first fluid source through the first distribution channel, the first port, and the first valve
  • the said second pressure buffer is connected to the second fluid source through the second distribution channel, the second port, and the second valve.
  • the said first distribution channel between the said first port and the said first pressure buffer has minimum one branching, and preferably from 2 to 10 branchings.
  • the said second distribution channel between the said second port and the said second pressure buffer has minimum one branching, and preferably from 2 to 10 branchings.
  • the said first valve is connected to the said first port through a tube with high hydraulic resistance, preferably a capillary
  • the said second valve is connected to the said second port through a tube with high hydraulic resistance, preferably a capillary.
  • the said microfluidic ju nctions ( 1 6) are T-junctions or flow- focusing junctions.
  • the device according to the invention has a sensor, preferably a camera, for monitoring the size of the d rop let generated in at least one of the said microfluidic junctions, connected directly or indirectly to at least one of the said valves.
  • the device additionally comprises n>2 microchannels originating at the third pressure buffer, con necting in pairs to the said n microcha n nels, prefera bly so that the connection results in n serially connected pairs of microfluidic T-junctions.
  • the present invention comprises also a method for high-throughput, on- demand generation of droplets, according to which the first fluid is passed through n>2 microchannels originating at the first pressure buffer, and the second fluid is passed through n corresponding microchannels, originating at the second pressure buffer, whereas the said microchannels meet in pairs in n microfluidic junctions, a nd the flow of the first fluid is controlled by the first pressure buffer, a nd that of the second fluid is controlled by the second pressure buffer.
  • the said first fluid, or the said second fluid is a fluid composed of two miscible or immiscible fluids.
  • droplets of two miscible fluids are generated sim u lta neously, a nd su bseq uently are merged, for instance using electric field, or with other methods of droplet coalescence known in the state of the art.
  • the said first pressure buffer is connected to the first fluid source through the first distribution channel, the first port, and the first valve
  • the said second pressure buffer is connected to the second fluid source through the second distribution channel, the second port, and the second valve
  • the said control of the flow of the first fluid by the first pressure buffer and that of the second fluid by the second pressure buffer is accomplished by opening and closing the said first valve and the said second valve, respectively.
  • a sensor is placed to monitor the size of droplets in that junction, preferably a camera, and the signal from the sensor is used to control operation of at least one of the said valves.
  • Fig.1 shows a schematic diagram of connections of the elements that are external to the system, in particular the placement of reservoirs with fluids, valves and hydraulic tubes,
  • Fig.2 presents a schematic diagram illustrating the arrangement of the channels in the system together with the inlets and the outlet, and with labelled T-junctions,
  • Fig.3 presents a characteristic of the system operation with 16 parallel junctions without valves (a) and with valves (b),
  • Fig.4 shows the dependence of the droplet size on the flow rate of the droplet phase in a system with 16 parallel junctions with triggering of the droplet valve closing operation by the camera (,, ⁇ " symbols) and without triggering (,,o"parallel junctions), and
  • Fig.5 presents a schematic diagram of a single junction and a system of parallel connected junctions for a single T-junction (a) and a double T-junction (b), and in the case when two miscible droplet phases are used (c).
  • the solution consists in providing a feedback to the valve controlling the droplet phase by the sig na l from the ca m era or a nother detection device providing information about the droplet volume.
  • the system described here (Fig. 1 ) is composed of external pressurised sources of fluids 1 , 2, valves 3, 4, tubes with high hydraulic resistance 5, 6 and the microfluidic system 7. External reservoirs with fluids 1 , 2 are directly connected to the computer controlled electromagnetic valves 3, 4. These valves are opened and closed according to a preset protocol. The outlet of each valve is connected to one of the two long tubes with high hydraulic resistance 5, 6, which supply fluids directly to the system. Each fluid is pumped into the system (Fig. 2) through round inlet holes 8, 9 to wide (0.8 mm) distribution channels 10, 1 1 forming a branched network. The purpose of these branches is to distribute evenly pressure. The outlets of the distribution channels are connected to elongated reservoirs 12, 13 that act as pressure buffers (one for each fluid) .
  • each microchannel 15 containing the continuous phase has a corresponding microchannel 14 containing the droplet phase.
  • the microchannels corresponding to each other meet at T-junctions 1 6 that are distant from the pressure buffers and have each a microchannel 1 7 draining fluids to the junction, where both phases flow jointly, with one of them in a form of droplets. Both phases leave the system through an atmospheric outlet 18.
  • T-junctions 1 6 that are distant from the pressure buffers and have each a microchannel 1 7 draining fluids to the junction, where both phases flow jointly, with one of them in a form of droplets. Both phases leave the system through an atmospheric outlet 18.
  • Droplet generation in junctions 16 is controlled by operation of the valves 3, 4.
  • the droplet phase is turned on for the time td while the continuous phase is turned off.
  • the droplet phase is turned off for the time t c and the continuous phase is turned on, and the cycle is completed.
  • the length of droplets L and the intervals L c between them in channels can be controlled by changing opening times of the valves (Fig.3b), td,o P en and t c ,o P en (abbreviated as td and t c ), as opposed to the situation without valves (Fig.3a), where the quantities, L and Lc, are both functions of volumetric flows, qd and q c .
  • the device allows also for designing a sequence of droplets with any volumes by appropriately selecting the opening times of the valves ⁇ (tdi,t c i), (td2,t C 2),...,(tdN,t C N) ⁇ .
  • the accuracy of reproduction of the above sequence of opening times in the form of a sequence of droplet volumes is determined separately for each droplet by the ratio At/td, wherein At is a delay related to a finite full opening or full closing time of the valve. In particular, it holds also td, t c > 2At.
  • the design of the system and in particular the use of tubes with high hydraulic resistance 5, 6, branched distribution channels 10, 11, pressure buffers 12, 13, and long supplying microchannels 14, 15 to the junctions 16, aims at an increased hydrodynamic resistance of the system, and consequently at minimised relative fluctuations of the resistance due to the presence of droplets in the system and imperfections in fabrication of the microchannels 10, 11, 14, 15. In this way, reduced fluctuations of the resistance translate into reduced fluctuations of the droplet size.
  • Increasing hydrodynamic resistances reduce the effect of fluctuations, but do not make the size of the droplets independent of the applied pressures. This goal can be reached only with a feedback, i.e., when the operation of the valves depends on the momentary size of the droplets.
  • the feedback consists in triggering the droplet valve to close with a signal from the camera at the time moment, when a droplet in the selected channel reaches the desired length.
  • the brightness threshold is set for a selected pixel in the camera, at a distance L from the junction, and when the threshold is exceeded it signals the emergence of the droplet-external phase interface.
  • the valve with the droplet phase is closed, the continuous phase is turned on and a droplet of a length L is generated. Due to the fact that the same valve is used to operate all parallel channels, droplets of identical length are produced simultaneously in all channels.
  • the method of device operation implies that the droplet monodispersity in time in a given channel is determined by the accuracy of the feedback operation. Due to the size of the channels 14, 15, however, an important role here plays also the design of the device, and in particular the precision of fabrication and the length of microchannels 14, 15, as well as the geometry of the pressure buffers 12, 13 inside the system, and the length of external tubes with high hydraulic resistance 5, 6.
  • the microfluidic system is composed of three polycarbonate sheets. Appropriately wide distribution channels 10, 1 1 , 0.8 mm wide, and microchannels 14, 15, 0.2 mm wide, together with the T-junctions 1 6 are milled in the upper and in the lower sheets, 2 and 5 mm thick, respectively.
  • the medium sheet separates the channels in both adjacent sheets, covering them at the same time, and has appropriately positioned through holes.
  • the system is bonded in a hydraulic press under pressure 1 ⁇ and a ⁇ temperature 130°C after prior modification of each plate in oxygen plasma.
  • valves 3, 4, one 4 controlling the continuous phase, and another one 3 - controlling the droplet phase, to operate many parallel connected junctions may be extended for the case of a greater number of valves, i.e., when one needs to introduce more than two phases into the system.
  • Introducing an additional phase to the system opens the possibility of, e.g., scanning the conditions of chemical reactions (single junction adapted for this purpose has been reported by K. Churski et al. in the Polish patent application No. P-390251, unpublished to date), or producing dual emulsions (an example of a passive system with single junction adapted for that purpose has been reported by N. Panacci et al., Physical Review Letters, 2008, 101, 104502).
  • phase C in phase B (junction TCB), i.e., C/B emulsion
  • TAA second junction
  • Fig. 5b an integrated system of multiple dual junctions
  • Fig. 5b the use is made of a dual T-junction of different type than the one used for generation of dual emulsions.
  • Miscible droplet phases B and C are independently supplied to the continuous phase A using two junctions TCA and TBA, giving rise to a pair of droplets C/A and B/A.
  • Such a pair of droplets can subsequently coalescence, for instance as a result of an applied electric field, generated by electrodes placed in the vicinity of the junction.
  • a corresponding system in an example of embodiment is illustrated in Fig.5c.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention porte sur un dispositif pour la production à haut débit à la demande de gouttelettes, caractérisé en ce qu'il comprend n>2 microcanaux (14) qui partent du premier tampon de pression (12) et n microcanaux correspondants (15), qui partent du second tampon de pression (13), alors que lesdits microcanaux (14, 15) se rejoignent par paires dans n jonctions microfluidiques (16). L'invention porte également sur un procédé pour la production à haut débit à la demande de gouttelettes, caractérisé en ce que le premier fluide est amené à passer dans n≥2 microcanaux (14) qui partent du premier tampon de pression (12) et le second fluide est amené à passer dans n microcanaux correspondants (15), qui partent du second tampon de pression (13), alors que lesdits microcanaux (14, 15) se rejoignent par paires dans n jonctions microfluidiques (16), et le débit du premier fluide est réglé par le premier tampon de pression (12) et celui du second fluide est réglé par le second tampon de pression (13).
PCT/EP2012/064641 2011-07-27 2012-07-25 Dispositif et procédé pour la production et la fusion à haut débit à la demande de gouttelettes WO2013014216A1 (fr)

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PL395775A PL221042B1 (pl) 2011-07-27 2011-07-27 Urządzenie i sposób do wysokoprzepustowego tworzenia i łączenia kropli na żądanie
PLP-395775 2011-07-27

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016010861A1 (fr) * 2014-07-14 2016-01-21 President And Fellows Of Harvard College Systèmes et procédés pour une performance améliorée de systèmes fluidiques et microfluidiques
EP3068526A2 (fr) * 2013-11-11 2016-09-21 King Abdullah University Of Science And Technology Dispositif microfluidique pour la production et le traitement à haut volume d'émulsions monodispersées
CN107638836A (zh) * 2017-11-09 2018-01-30 东南大学 一种多重乳液制备系统
WO2019074951A1 (fr) * 2017-10-09 2019-04-18 Altopa, Inc. Dispositif microfluidique portatif sécurisé, à la demande, pour mélanger et distribuer des mélanges de liquides, de solutions, de suspensions, d'émulsions et de colloïdes
CN115254222A (zh) * 2022-07-19 2022-11-01 天津大学 基于非对称并行微通道制备单分散非牛顿流体液滴的方法
US11666875B2 (en) 2016-04-11 2023-06-06 Altopa, Inc. Secure portable, on-demand, microfluidic mixing and dispensing device
EP4159305A3 (fr) * 2021-09-10 2023-06-07 Suzhou Precigenome Ltd, Co; Système microfluidique de synthèse de nanoparticules, et dispositif et procédé l'utilisant

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WO2010104597A2 (fr) * 2009-03-13 2010-09-16 President And Fellows Of Harvard College Mise à l'échelle de dispositifs microfluidiques
PL390251A1 (pl) 2010-01-24 2011-08-01 Instytut Chemii Fizycznej Polskiej Akademii Nauk Metoda i układ do wytwarzania kropli na żądanie w układzie mikroprzepływowym oraz tworzenia sekwencji kropli o arbitralnie zadanych kombinacjach stężeń roztworów wejściowych

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3068526A2 (fr) * 2013-11-11 2016-09-21 King Abdullah University Of Science And Technology Dispositif microfluidique pour la production et le traitement à haut volume d'émulsions monodispersées
EP3068526B1 (fr) * 2013-11-11 2021-05-05 King Abdullah University Of Science And Technology Dispositif microfluidique pour la production et le traitement à haut volume d'émulsions monodispersées et procédé
GB2546424A (en) * 2014-07-14 2017-07-19 Harvard College Systems and methods for improved performance of fluidic and microfluidic systems
WO2016010861A1 (fr) * 2014-07-14 2016-01-21 President And Fellows Of Harvard College Systèmes et procédés pour une performance améliorée de systèmes fluidiques et microfluidiques
US10407655B2 (en) 2014-07-14 2019-09-10 President And Fellows Of Harvard College Systems and methods for improved performance of fluidic and microfluidic systems
US11034926B2 (en) 2014-07-14 2021-06-15 President And Fellows Of Harvard College Systems and methods for improved performance of fluidic and microfluidic systems
US11434458B2 (en) 2014-07-14 2022-09-06 President And Fellows Of Harvard College Systems and methods for improved performance of fluidic and microfluidic systems
US11666875B2 (en) 2016-04-11 2023-06-06 Altopa, Inc. Secure portable, on-demand, microfluidic mixing and dispensing device
WO2019074951A1 (fr) * 2017-10-09 2019-04-18 Altopa, Inc. Dispositif microfluidique portatif sécurisé, à la demande, pour mélanger et distribuer des mélanges de liquides, de solutions, de suspensions, d'émulsions et de colloïdes
CN107638836A (zh) * 2017-11-09 2018-01-30 东南大学 一种多重乳液制备系统
CN107638836B (zh) * 2017-11-09 2023-10-03 东南大学 一种多重乳液制备系统
EP4159305A3 (fr) * 2021-09-10 2023-06-07 Suzhou Precigenome Ltd, Co; Système microfluidique de synthèse de nanoparticules, et dispositif et procédé l'utilisant
CN115254222A (zh) * 2022-07-19 2022-11-01 天津大学 基于非对称并行微通道制备单分散非牛顿流体液滴的方法
CN115254222B (zh) * 2022-07-19 2023-11-07 天津大学 基于非对称并行微通道制备单分散非牛顿流体液滴的方法

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