WO2011091342A1 - Microréacteurs à dispositif microfluidique et application d'ultrasons au niveau du système; mise en œuvre de réactions chimiques dans lesdits microréacteurs - Google Patents

Microréacteurs à dispositif microfluidique et application d'ultrasons au niveau du système; mise en œuvre de réactions chimiques dans lesdits microréacteurs Download PDF

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Publication number
WO2011091342A1
WO2011091342A1 PCT/US2011/022196 US2011022196W WO2011091342A1 WO 2011091342 A1 WO2011091342 A1 WO 2011091342A1 US 2011022196 W US2011022196 W US 2011022196W WO 2011091342 A1 WO2011091342 A1 WO 2011091342A1
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Prior art keywords
microfluidic device
microreactor
transducer
joined
ultrasound
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PCT/US2011/022196
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English (en)
Inventor
Carine Cerato-Noyerie
Sylvain Maxime F. Gremetz
Clemens R. Horn
Olivier Lobet
Pierre Woehl
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Corning Incorporated
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Publication of WO2011091342A1 publication Critical patent/WO2011091342A1/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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00824—Ceramic
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00831—Glass
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00835—Comprising catalytically active material
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/0086—Dimensions of the flow channels
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00889—Mixing
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00925—Irradiation
    • B01J2219/00932—Sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components

Definitions

  • the present invention relates to: microreactors incorporating a planar micro fluidic device and an ultrasonic application system in their structure. Said microreactors are able to exist according to two main alternatives:
  • microreactors equipped with empty housings (receptacles), for the stable positioning within them of such means for said ultrasound application; and the use of said microreactors, more particularly methods for carrying out chemical reactions within said microreactors.
  • the present invention has been developed in particular with reference to chemical reactions generating solids, which are liable to clog the channels of the microfluidic device and/or to sono-chemical reactions.
  • its field of application is not limited to these contexts.
  • microfluidic devices of the microreactors of the invention are fluidic devices of which the channels (for fluid flow) have their smallest dimension between a few tens of microns and a few millimetres, generally between 100 microns and 2 millimetres.
  • US Patent No. 7,007,709 discloses such microfluidic devices and a process for manufacturing them.
  • At least one transducer is placed inside said microstructure; (2) prepare mixtures efficiently: in this respect, mention can be made in particular of the following teachings: (a) patent application US-A-2008/0049545 : a porous material is arranged in a vessel. At least one ultrasonic actuator is arranged on at least one wall of said vessel.
  • patent US 7 401 970 feed tubes of a microstructure, intended to be joined within said microstructure, are vibrated by ultrasonic action, outside said microstructure (upstream of their junction in said microstructure);
  • patent application US-A-2009/0043122 a high quality dispersion is generated in a delay microreactor, and ultrasonic action is used for this purpose;
  • patent application US 2006/0034735 ultrasound is applied within a microstructure, locally, slightly downstream of the junction of two channels, directly on the junction channel (internal application);
  • PCT patent publication WO 2004/030800 ultrasound is also applied here locally; it is more precisely applied to a junction of two channels, from the outer surface of the microstructure (external application), and a very high frequency is required, 6 to 200 Mz, for a maximum distance between said outer surface where the ultrasound is generated (where the transducer is bonded) and the junction of the two
  • the inventors propose an original microreactor concept, with planar microfluidic device and ultrasonic application system.
  • the planar microfluidic device is equipped with the ultrasound application system. It is ready for use (as such or with further arrangements: positioning of at least one additional transducer in at least one empty housing provided for this purpose (see below));
  • the planar microfluidic device is not equipped with the ultrasound application system but with means ready to accommodate said system.
  • This modular approach is particularly advantageous, especially with reference to the problem of the fragility of said ultrasound application system and to the possible and completely independent replacement of said ultrasound application system and said planar microfluidic device.
  • Said concept is efficient. It notably allows the implementation of chemical reactions within original microreactors, under advantageous conditions (see below).
  • the primary object of the present invention therefore concerns microreactors, of which the structure comprises a microfluidic device and at least one transducer (ultrasound application system). Characteristically:
  • said microfluidic device is a planar microfluidic device
  • the volume is bounded by an outer surface formed by at least one side face having a low height h and by two substantially parallel main faces, of which the smallest dimension 1 is such that h/1 ⁇ 10 1 , of which the internal volume for circulating at least one fluid (fluid to treat within said internal volume) is higher than 0.35 ml; the shortest distance e between said outer surface and the proximal zone of said internal volume being at least 400 ⁇ ; and, said at least one transducer for vibrating said microfluidic device in its whole volume, is joined to said outer surface of said microfluidic device.
  • Said ratio h/1 is lower than 10 "1 , such that the microfluidic device is a planar, and not a tubular one.
  • the ratio is lower than 10 ⁇ 2 (h/1 ⁇ 10 ⁇ 2 ).
  • it is between 10 ⁇ 3 and 10 "2 (10 3 ⁇ h/1 ⁇ 10 "2 ).
  • said microfluidic device has a low height h equal to or lower than 12 mm.
  • This height h, of its side walls or of its side wall, is advantageously between 3 and 9 mm.
  • the internal volume of said microfluidic device is "substantial", higher than 0.35 ml.
  • said internal volume is generally higher than 0.5 ml, or even higher than 1 ml, or even still higher than 5 ml.
  • said internal volume, v is between 6 and 20 ml: 6 ml ⁇ v ⁇ 20 ml.
  • the material constituting said microfluidic device is selected from glass, vitroceramic and ceramic.
  • the thickness of this constituent material between the outer surface and the internal volume of said microfluidic device is at least 400 ⁇ . It is generally at least 450 ⁇ , or even at least 500 ⁇ . It can be stated here, in a non-limiting manner, that said distance e is generally lower than 5 mm. It is generally better to speak of the shortest distance e insofar as said microfluidic device is not necessarily symmetrical.
  • said shortest distance e is obviously related to the exact structure of the microfluidic device, structure with one or more fluid flow layers, whether symmetrical or not.
  • the microfluidic device generally comprises 1 to 4 fluid flow layers. It may comprise a single flow layer for fluid(s) (reaction fluid(s), for example). On this assumption, it may or may not have a symmetrical structure. When it has a symmetrical structure, the same distance e is then found on either side of its axis of symmetry.
  • Said microfluidic device may also comprise one flow layer for fluid(s) (reaction fluid(s), for example) and at least one flow layer for a heat exchange fluid.
  • reaction fluid(s), for example a flow layer for fluid(s) (reaction fluid(s), for example) between two layers intended for the flow of a heat exchange fluid.
  • the structure of said microfluidic device may also be symmetrical or not.
  • Other alternative structures of said microfluidic device are obviously possible, for example at least two layers for the flow of fluid(s) (reaction fluid(s), for example). It may be observed here incidentally that, in a context of chemical reaction, at least two reaction fluids (required to react with one another) are generally circulated in said microfluidic device, but it is not inconceivable that a single fluid containing a single reactant (reactive under the action of light or heat, for example) or containing several reactants may be circulated.
  • the planar microfluidic device having the features described above, is equipped according to the invention with at least one transducer.
  • said at least one transducer is arranged on the outer surface of said planar microfluidic device (it is not part of the internal structure of said planar microfluidic device; there is no contact between the fluid(s) flowing in said internal structure and said at least one transducer) and it is suitable for vibrating said planar microfluidic device in its whole volume (its action is not localized).
  • the planar microfluidic device which is an essential component of the structure of the microreactors of the invention, is of the type of those developed in recent years by the Applicant, and, totally surprisingly, without any modification of its characteristics (particularly geometrical characteristics), its combination, according to the invention, with at least one transducer (other essential component of the structure of the microreactors of the invention), enables said at least one transducer to develop an effective action without weakening, or even breaking, said planar microfluidic device. It is this combination - planar microfluidic device having the characteristics described above + at least one transducer, joined to the surface and suitable for vibrating it in its whole volume - which constitutes the basis of the present invention.
  • the structure of the microreactors of the invention thus comprises a microfluidic device as described above and at least one transducer on the surface of said microfluidic device, suitable for vibrating said microfluidic device in its whole volume.
  • Said structure advantageously comprises at least two transducers.
  • Said at least two transducers may both be arranged on the same main face of the microfluidic device or may be distributed on the two main faces of said microfluidic device (in which case at least one transducer is joined to each of the two main faces of the outer surface of the microfluidic device). It is thus clearly possible to optimize the action of the ultrasound in the volume of the microfluidic device by adjusting the number and arrangement of the transducers.
  • the height h of the microfluidic device (the thickness of said microfluidic device) is great. This may be highly advantageous in the structure of a microreactor with multilayer microfluidic device.
  • a microfluidic device which (substantially) has the shape of a parallelogram or a circle, it is advantageous for them to be arranged along a diagonal or along a diameter. It is highly advantageous for them to be thus arranged along a diagonal or along a diameter, spaced by a distance at least equal to 5 times the low height h of the microfluidic device.
  • the at least one transducer there is a junction between said at least one transducer and said outer surface of said microfluidic device.
  • This junction may be direct or indirect, via for example a means, itself joined to said outer surface of said microfluidic device and suitable for accommodating a transducer.
  • a means is of the resonating housing type insofar as it must be suitable for the stable positioning within itself of a transducer and for the transmission of ultrasound.
  • Said housing is provided to accommodate a single transducer within itself.
  • Said housing may in particular consist of a metal part (of aluminium, for example) with a recess in its mass, adapted to the dimensions of the transducer.
  • the transducer may be positioned in a stable manner in said housing, by screwing. [0028]
  • the transducer, positioned in a housing, is protected. This alternative of the microreactors of the invention, with housing(s) for the transducer(s) present, is particularly preferred.
  • the microreactors of the invention equipped with at least one transducer, joined directly or indirectly via a resonating housing, may perfectly well also be equipped with at least one empty resonating housing, suitable for accommodating another transducer, if required.
  • the person skilled in the art will not fail to grasp the flexibility of use that is thereby conferred on the microreactors of the invention.
  • the microreactor of the invention comprises, in its structure, at least one transducer (generally transducers) arranged in a housing (arranged in housings);
  • the microreactor of the invention comprises, in its structure, at least one transducer (generally transducers) arranged in a housing (arranged in housings) and at least one other empty housing.
  • the direct joining (transducer(s)/outer surface of the microfluidic device) or indirect joining (resonating housing(s)/outer surface of the microfluidic device) is advantageously carried out by bonding.
  • the glue employed (the glue joint involved) is obviously suitable for the bonding (constituent material of the microfluidic device (glass, vitroceramic, ceramic)/constituent material of the transducers or of the housings (metal, for example)) and for transmitting the ultrasound (without significant deterioration of its mechanical properties).
  • microreactors of the invention described above are equipped with an ultrasound application system (primary object of the invention)and so are ready (or virtually ready) for use.
  • the invention also relates (second object of the invention) to planar microfluidic devices, not yet equipped with an ultrasound application system but with means ready for accommodating such a system, able for vibrating said microfluidic device in its whole volume.
  • Such reactors, precursors of the aforementioned ready-to-use (or virtually ready-to-use) microreactors are an integral part of the invention.
  • said microfluidic device is a planar microfluidic device made from glass, vitroceramic or ceramic, of which the volume is bounded by an outer surface formed by at least one side face having a low height h and by two substantially parallel main faces , of which the smallest dimension 1 is such that h/1 ⁇ 10 "1 , of which the internal volume (v) for circulating at least one fluid is higher than 0.35 ml; the shortest distance e between said outer surface of the microfluidic device and the proximal zone of said internal volume (v) being at least 400 ⁇ ; and, at least one (empty) housing made from an ultrasound-conducting material, suitable for the stable positioning within it of at least one transducer, is joined to said outer surface of said microfluidic device.
  • Said planar microfluidic device is such as described above with reference to the microreactors equipped with at least one transducer.
  • planar microfluidic device is associated here with at least one housing for transducer.
  • At least two housings are joined to the outer surface of the planar microfluidic device
  • At least two housings are joined to the same main face of the outer surface of the planar microfluidic device;
  • said at least two housings joined to the same main face are advantageously spaced at a distance at least equal to 5 times the low height h;
  • said main face substantially having, respectively, the shape of a parallelogram or a circle, said at least two housings, joined to said main face are advantageously respectively arranged along a diagonal or along a diameter;
  • At least one housing is joined to each of the two main faces of the outer surface of the microfluidic device; the joining is provided by a glue joint.
  • microreactors of the invention ready to accommodate at least one transducer, are particularly advantageous. They can be equipped, at the last moment (just before use), with at least one transducer; they can be equipped, as desired, with one or more transducers, according to the housings provided. This leaves considerable leeway for action and optimization, according to the precise intended use. As stated above, they are also particularly advantageous with reference to the fragility of their constituent components, microfluidic device/transducer(s), with reference to the possibility of replacing each of these elements (in an independent manner).
  • microreactors of the invention equipped or ready to be equipped with at least one transducer.
  • the use of said microreactors, in general - the method for carrying out a chemical reaction within them, in particular - is moreover advantageous. It constitutes the final object of the present invention.
  • Said method for carrying out a chemical reaction comprises the following steps: procuring a microreactor according to the first object of the invention, that is as described above: equipped with at least one transducer, or procuring a microreactor according to the second object of the invention, that is as described above: equipped with at least one empty housing and then positioning a transducer in said empty housing or in at least one of said empty housings; circulating at least one reactive fluid (generally a mixture of at least two reactive fluids) in the internal volume of said microreactor equipped with at least one transducer; the circulating advantageously occurs at a flow rate equal to or higher than 1 ml/min (with reference to the channel clogging problem); actuating the transducer present or at least one of the transducers present (generally at least two transducers are present) at a nominal frequency of between 1 and 200 kHz, advantageously about 50 kHz, to deliver a power density of at least 0.1 MW/m 3 , in order to vibrate said microfluidic
  • the action of the transducers is not limited to a localized one (or to localized ones). It consists in the vibration of the microfluidic device in its whole volume. So there is no constraint at all related to coupling between the position(s) of the transducer(s) and the design, arrangement, or layout of the microfluidic channels within the microfluidic device.
  • the actuation of at least one transducer to be actuated can generally be carried out in continuous mode or in pulse mode, optionally with a frequency sweep around the nominal frequency.
  • the method of the invention is advantageously implemented (the microreactors of the invention are advantageously employed) in the following contexts: chemical reactions generating solids; the ultrasound then being generated (by said at least one transducer joined directly or indirectly to the outer surface of the planar microfluidic device) to delay or even prevent the clogging in the internal volume (the channels) of the microfluidic device; sono- chemical reactions, in particular sono-crystallization reactions.
  • microreactors of the invention are advantageously employed in contexts which include operations of mixing, separation, extraction, crystallization, precipitation, or any other operation conducted on fluids or fluid mixtures (including mixtures of fluids in several phases; fluids or fluid mixtures, possibly with several phases, laden with solids).
  • the concerned operations are able to imply a physical process, a chemical reaction defined as a method resulting in a conversion of species, organic, inorganic, or both organic and inorganic, a biochemical method, or any other type of method.
  • any reaction of the non-exhaustive list below can be implemented with the microreactors and/or methods of the invention: polymerization; alkylation; dealkylation; nitration; peroxydation; sulphoxidation; epoxidation; ammoxidation; hydrogenation; dehydrogenation; organometalic reactions; chemistry of precious metals/homogeneous catalyst reactions; carbonylation; thiocarbonylation; alkoxylation; halogenation; dehydrohalogenation; dehalogenation; hydroformylation; carboxylation; decarboxylation; amination; arylation; coupling of peptides; aldol condensation; cyclocondensation; dehydrocyclization; esterification; amidation; heterocyclic synthesis; dehydration; alcoholysis
  • Figure 1 schematically shows a cross section of a microreactor of the invention equipped with two transducers.
  • Figure 2A schematically shows a cross section of another microreactor of the invention also equipped with two transducers.
  • Figure 2B schematically shows a cross section of another microreactor of the invention, similar to the one in Figure 2A, not equipped with transducers but equipped with two housings each suitable for accommodating a transducer.
  • Figure 3 A shows a perspective view of a microreactor of the invention, with type 1 microfluidic device (with a single fluid flow layer), not equipped with transducers but equipped with five housings each suitable for accommodating a transducer.
  • Figure 3B shows a perspective view of the microreactor of Figure 3A equipped with two transducers.
  • Figure 4 shows the results of tests conducted on the microreactor of Figure 3B (with type 1 microfluidic device), used for carrying out two chemical reactions. These tests are explained in Example 1 below. The rise in pressure in the channels is monitored as a function of time.
  • Figure 5 also shows the results of tests conducted on the microreactor of Figure 3B (with type 1 microfluidic device), used for carrying out a chemical reaction. Said tests are explained in Example 1 below. The pressure rise in the channels is monitored as a function of time, at various ultrasonic powers (0 to 10 W).
  • Figure 6 shows another microreactor of the invention, with type 2 micro fluidic device (with a plurality of fluid flow layers), equipped, like the microreactor with type 1 microfluidic device of Figure 3B, with two transducers.
  • Figure 7 shows the variation in clogging time, during the carrying out of a reaction, as a function of the ultrasonic power applied, for a microreactor with type 1 microfluidic device (Figure 3B) and a microreactor with type 2 microfluidic device (Figure 6). It is commented on in Example 1 below.
  • Figure 8 shows another microreactor of the invention with type 3 microfluidic device (with a single fluid flow layer), equipped, like the microreactor with type 1 fluidic device of Figure 3B and the microreactor with type 2 microfluidic device of Figure 6, with two transducers.
  • Figures 9A and 9B show, at two different flow rates, the increase in pressure as a function of time in the channels of the type 3 microfluidic device, used for carrying out a chemical reaction. The test is explained in Example 2 below.
  • the microreactor 10 of the invention shown schematically in Figure 1, has a structure which can be qualified as a basic structure.
  • Said basic structure comprises:
  • a planar microfluidic device 1 1 which has a single flow layer 7 for reactive fluid(s).
  • Said microfluidic device 1 1 is of the type described in international application WO 2008/106160 (obtained by sealing, using a glass frit, glass portions).
  • Said microfluidic device is planar. Its volume is bounded by its outer surface 6, formed by at least one side face 6c having a low height h and two substantially parallel main faces 6a and 6b.
  • the said device 1 1 is for example parallelepipedic or cylindrical, and all events, has a low thickness: h is at least ten times lower than the smallest dimension of said two faces 6a and 6b (these faces being square, rectangular or circular, for example).
  • Its internal volume v (higher than 0.35 ml) consists of at least one flow channel 4.
  • Zone 4' is qualified as proximal;
  • the microfluidic device 21 comprises three fluid flow layers: layer 7 for the flow of the at least one reactive fluid, layers 7' and 7", on either side of the said layer 7, for the flow of a heat exchange fluid. Its thickness h remains low.
  • the heat exchange fluid(s) flow(s) in the channels 5.
  • the device 21 was in particular obtained using the technique described in patent application US 2004/0206391.
  • the transducers 1 were arranged in resonating housings 3. Said housings 3 are bonded (using a glue transparent to ultrasound) to the outer surface 6 of the device 21.
  • a transducer 1 is found in its housing 3 on each of the main faces, respectively 6a and 6b, of the surface 6.
  • the distance e here is observed with reference to each of the faces 6a and 6b of the outer surface 6 of the device 21. It encompasses a heat exchange fluid flow layer: 7 " on the side of face 6a, 7' on the side of face 6b.
  • a symmetrical structure is shown, but it would not be inconceivable for e to be on the face 6a side (shown in Figure 2A) and e' on the face 6b side (not shown in Figure 2A) to be different.
  • the microfluidic device of the microreactors of the invention is vibrated in its whole volume by the action of ultrasound, through thicknesses higher than 400 ⁇ .
  • the microreactor 60 in Figure 2B is similar to the one 20 in Figure 2A. However, the resonating housings 3 ' are empty. The transducers are not (yet) arranged therein. [0066]
  • the microreactor 60 is an "intermediate product", to be equipped for its use, with at least one transducer. It may be equipped with two transducers, each positioned in a housing 3 '.
  • the microreactor 70 in Figure 3A is also a microreactor of the invention not (yet) equipped with at least one transducer 1. Joined to the outer surface 6, more precisely to one of the main faces of said outer surface 6, with its planar micro fluidic device 31, there are five (empty) housings 3 ', each capable of accommodating such a transducer 1. Said microreactor 70 may therefore easily, before use, be equipped, as desired, with one, two, three, four or five transducers. The dotted arrows evoke these possibilities.
  • the microfluidic device 31 of said microreactor 70 a type 1 device (with reference to the design of its internal volume), comprises a single fluid flow layer.
  • Figure 3A is a perspective view. This figure shows the smallest dimension 1 of the microfluidic device 31. This smallest dimension 1 is more than ten times higher than the thickness h of the said microfluidic device 3 1. Said microfluidic device 31 is a planar microfluidic device.
  • the microreactor 30 in Figure 3B corresponds to the microreactor 70 in Figure 3A equipped with two transducers 1. Said two transducers 1 have been positioned in two housings 3 ' arranged, one after the other, along a diagonal of the microfluidic device 3 1 (type 1). Reference numeral 3 denotes said two occupied housings and also 3 ' those which have remained empty.
  • This microreactor 30 was tested, in particular with the carrying out therein of the (non-balanced) reaction below, forming a cuprous hydroxide precipitate: CuCl 2 + NaOH -> Cu(OH) 2 ; hence the representation in Figure 3B of the CuCl 2 and NaOH feeds.
  • the features of said microreactor 30 and the test conditions are indicated below in connection with Example 1.
  • the test results are shown in Figures 4 and 5. They are commented on in said Example 1.
  • the microreactor 40 in Figure 6 comprises a planar microfluidic device 41 with a fluid flow layer according to a particular design between two flow layers of a heat exchange fluid: H 2 0.
  • Said microfluidic device 41 is referenced as a type 2 microfluidic device. It is equipped on its outer surface, on one of its main faces, with five housings for transducers, two 3 occupied and three 3 ' empty.
  • microreactor 40 was tested for the reaction indicated above, in parallel with the microreactor 30 in Figure 3B, at different ultrasonic powers. The characteristics of said microreactor 40 and the test conditions are indicated below in connection with Example 1.
  • the microreactor 50 in Figure 8 comprises a planar microfluidic device 51 with a
  • microfluidic device 51 is referenced as a type 3 microfluidic device. It is equipped on its outer surface, on one of its main faces, with five housings for transducers, two 3 occupied and three 3 ' empty.
  • microreactor 51 was tested, with precipitation therein of sodium sulphate decahydrate.
  • the characteristics of said microreactor 51 and the test conditions are indicated below in connection with Example 2.
  • the test results, conducted at two different flow rates, are shown respectively in Figures 9A and 9B. They are commented on in said Example 2.
  • Said microfluidic devices are equipped with two cylindrical piezoelectric ceramic transducers (comprising a thread on their outer surface), sold by STNAPTEC.
  • Said cylindrical transducers have an imprint of 16 x 16 mm 2 (256 mm 2 ) and a height of 10 mm.
  • Said two transducers are positioned as shown in the figures, along the diagonal of the microfluidic devices, one after the other. They are positioned by screwing in the housings, having a recess with threads (hollow, with dimensions adapted to those of said transducers).
  • Said housings are aluminium metal cubes.
  • the glue used is a two-component thixotropic adhesive, transmitting the ultrasound.
  • reaction 1 was carried out in a microreactor, as shown in Figure 3B, without ultrasound applied (0 W) and with ultrasound applied at various powers (2 to 10 W).
  • the effectiveness of said ultrasound is confirmed. It varies in a linear manner with the power applied: see said Figure 5 and the lower curve (right) in Figure 7.
  • the time after which the clogging is observed increases in a linear manner with said power applied in the microreactor - type 1 microfluidic device + two transducers - shown in Figure 3B.
  • microreactor has one side face with a greater height h, insofar as it contains three layers. It is also stated that water fills the outer flow layers. The same results are expected with the circulating of said water in said outer flow layers at a flow rate of 300 g/min or more.
  • Figures 9A and 9B clearly demonstrate the gain, in terms of operating time, for a planar microfluidic device with application of ultrasound according to the invention.

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

Abstract

La présente invention concerne des microréacteurs (30), dont la structure comprend un dispositif microfluidique plan (31) en verre, vitrocéramique ou céramique et au moins un transducteur (1), destiné à faire vibrer l'intégralité du volume dudit dispositif microfluidique (31) et relié à la surface extérieure (6) de ce dernier (31); des microréacteurs, dont la structure comprend un tel dispositif microfluidique plan équipé d'au moins un boîtier (3') constitué d'un matériau conduisant les ultrasons, et dans lequel peut être positionné de façon stable un transducteur (1), relié à ladite surface extérieure (6) dudit dispositif microfluidique. L'invention concerne également des procédés de mise en œuvre de réactions chimiques faisant appel auxdits microréacteurs.
PCT/US2011/022196 2010-01-25 2011-01-24 Microréacteurs à dispositif microfluidique et application d'ultrasons au niveau du système; mise en œuvre de réactions chimiques dans lesdits microréacteurs WO2011091342A1 (fr)

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FR1050459A FR2955508B1 (fr) 2010-01-25 2010-01-25 Microreacteurs avec dispositif microfluidique plan et systeme d'application d'ultrasons ; mise en oeuvre de reactions chimiques en leur sein
FR10/50459 2010-01-25

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115253833A (zh) * 2021-04-30 2022-11-01 华东理工大学 一种用于混合微流体的微型混合装置

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EP1179585A2 (fr) 1997-12-24 2002-02-13 Cepheid Cartouche de manipulation de fluide intégrée
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