This application claims priority to European Patent Application Number 08305711.7, filed Oct. 22, 2008 and European Patent Application Number 08305610.1 filed Sep. 29, 2008, titled “Multiple Flow Path Microreactor Design”.
Microfluidic devices, as understood herein, include fluidic devices over a scale ranging from microns to a few millimeters, that is, devices with fluid channels the smallest dimension of which is in the range of microns to a few millimeters, and preferably in the range of from about 10's of microns to about 2 millimeters. Partly because of their characteristically low total process fluid volumes and characteristically high surface to volume ratios, microfluidic devices, particularly microreactors, can be useful to perform difficult, dangerous, or even otherwise impossible chemical reactions and processes in a safe, efficient, and environmentally-friendly way. Such improved chemical processing is often described as “process intensification.”
Process intensification is a paradigm in chemical engineering which has the potential to transform traditional chemical processing, leading to smaller, safer, and more energy-efficient and environmentally friendly processes. The principal goal of process intensification is to produce highly efficient reaction and processing systems using configurations that simultaneously significantly reduce reactor sizes and maximize mass- and heat-transfer efficiencies. Shortening the development time from laboratory to commercial production through the use of methods that permit the researcher to obtain better conversion and/or selectivity is also one of the priorities of process intensification studies. Process intensification may be particularly advantageous for the fine chemicals and pharmaceutical industries, where production amounts are often smaller than a few metric tons per year, and where lab results in an intensified process may be relatively easily scaled-out in a parallel fashion.
Process intensification consists of the development of novel apparatuses and techniques that, relative to those commonly used today are expected to bring very important improvements in manufacturing and processing, substantially decreasing equipment-size to production-capacity ratio, energy consumption and/or waste production, and ultimately resulting in cheaper, sustainable technologies. Or, to put this in a shorter form: any chemical engineering development that leads to a substantially smaller, cleaner, and more energy efficient technology is process intensification.
The methods and/or devices disclosed herein are generally useful in performing any process that involves mixing, separation, extraction, crystallization, precipitation, or otherwise processing fluids or mixtures of fluids, including multiphase mixtures of fluids—and including fluids or mixtures of fluids including multiphase mixtures of fluids that also contain solids—within a microstructure. The processing may include a physical process, a chemical reaction defined as a process that results in the interconversion of organic, inorganic, or both organic and inorganic species, a biochemical process, or any other form of processing. The following non-limiting list of reactions may be performed with the disclosed methods and/or devices: oxidation; reduction; substitution; elimination; addition; ligand exchange; metal exchange; and ion exchange. More specifically, reactions of any of the following non-limiting list may be performed with the disclosed methods and/or devices: polymerisation; alkylation; dealkylation; nitration; peroxidation; sulfoxidation; epoxidation; ammoxidation; hydrogenation; dehydrogenation; organometallic reactions; precious metal chemistry/homogeneous catalyst reactions; carbonylation; thiocarbonylation; alkoxylation; halogenation; dehydrohalogenation; dehalogenation; hydroformylation; carboxylation; decarboxylation; amination; arylation; peptide coupling; aldol condensation; cyclocondensation; dehydrocyclization; esterification; amidation; heterocyclic synthesis; dehydration; alcoholysis; hydrolysis; ammonolysis; etherification; enzymatic synthesis; ketalization; saponification; isomerisation; quaternization; formylation; phase transfer reactions; silylations; nitrile synthesis; phosphorylation; ozonolysis; azide chemistry; metathesis; hydrosilylation; coupling reactions; and enzymatic reactions.
The present inventors and/or their colleagues have previously developed various microfluidic devices useful in process intensification and methods for producing such devices. These previously developed devices include apparatuses of the general form shown in prior art
The terms “horizontal” and “vertical,” as used in this document are relative terms only and indicative of a general relative orientation only, and do not necessarily indicate perpendicularity, and are also used for convenience to refer to orientations used in the figures, which orientations are used as a matter of convention only and not intended as characteristic of the devices shown. The present invention and the embodiments thereof to be described herein may be used in any desired orientation, and horizontal and vertical walls need generally only be intersecting walls, and need not be perpendicular.
A reactant passage 26, partial detail of which is shown in prior art
The reactant passage 26 has a constant height in a direction perpendicular to the generally planar walls.
The device shown in
In
Each of such chamber 34 includes a split of the reactant passage into at least two sub-passages 36, and a joining 38 of the split passages 36, and a change of passage direction, in at least one of the sub-passages 36, of at least 90 degrees relative to the immediate upstream passage direction. In the embodiment shown, it may be seen in
Also in the embodiment of
Although good performance has been obtained with devices of this type, in many cases even exceeding the state of the art for a given reaction, it has nonetheless become desirous to improve fluid dynamic performance. In particular, it is desirable to obtain a controlled and well-balanced residence time while simultaneously decreasing the pressure drop caused by the device, while increasing throughput.
In U.S. Pat. No. 7,241,423 (corresponding to US2002106311), “Enhancing fluid flow in a stacked plate microreactor,” parallel channels (see
A microfluidic device comprises at least one reactant passage (26) defined by walls and comprising at least one parallel multiple flow path configuration, said parallel multiple flow path configuration comprising a group of elementary design patterns of the flow path which are arranged in series with fluid communication so as to constitute flow paths, and in parallel so as to constitute a multiple flow path elementary design pattern in the parallel flow paths, said elementary design pattern being able to provide mixing and/or residence time, wherein the parallel multiple flow path configuration comprises at least two communicating zones between elementary design patterns of two adjacent parallel flow paths, said communicating zones being in the same plane as that defined by said elementary design patterns between which said communicating zone is placed and allowing passage of fluid (flow interconnections) in order to minimize mass flow rate difference between adjacent parallel flow paths which have the same flow direction.
In some cases, an equalization of the mass flow rate (and also of the fluid pressure) between the adjacent parallel flow paths of the parallel multiple flow path configuration can be achieved.
Moreover, this solution allows, thanks to the communicating zones, a uniformity of Residence Time in several parallel micro channels or flow paths of each parallel multiple flow path configuration.
Therefore, provided each flow path is of equal length, width and height to get a constant residence time and hydraulic properties, the parallel multiple flow path configuration according to the invention bring an increased of microreactor chemical production throughput.
Additional features and advantages of the invention will be set forth in the detailed description which follows, and in part will be readily apparent to those skilled in the art from that description or recognized by practicing the invention as described herein, including the detailed description which follows, the claims, as well as the appended drawings.
It is to be understood that both the foregoing general description and the following detailed description present embodiments of the invention, and are intended to provide an overview or framework for understanding the nature and character of the invention as it is claimed. The accompanying drawings are included to provide a further understanding of the invention, and are incorporated into and constitute a part of this specification. The drawings illustrate various embodiments of the invention, and together with the description serve to explain the principles and operations of the invention.
Reference will now be made in detail to the presently preferred embodiments of the invention, examples of which are illustrated in the accompanying drawings. Whenever possible, the same reference numerals will be used throughout the drawings to refer to the same or like parts.
Without limitation, in the microfluidic devices of the invention the reactant passage and its portion constituted by parallel multiple flow path configurations are generally extending in an horizontal plane and defined by vertical walls. The “width” refers to a direction which is perpendicular to the flow direction and parallel to said horizontal plane of the parallel multiple flow path configuration. The “heigth” refers to a direction which is perpendicular to the flow direction and perpendicular to said horizontal plane of the parallel multiple flow path configuration. The “length” refers to a direction which is parallel to the flow direction and parallel to said horizontal plane of the parallel multiple flow path configuration.
In
The two parallel path flows 52 are adjacent to each other. Also the adjacent chambers 34 of the two parallel path flows 52 form pairs of chambers 34 (more generally a multiple flow path elementary design pattern 57 with a communicating zone 54 between them. This communicating zone 54 is formed by a direct fluid connection between the pairs of chambers 34 so that when the flow of fluid passes in parallel in the two parallel path flows 52, there is a possible passage of fluid between the two parallel path flows 52 at the location of these communicating zone 54. Therefore, there is a contact point (common portion of wall) with an aperture/opening (communicating zone 54) between the adjacent chambers 34 of the parallel path flows 52.
This specific possible passage of fluid or flow interconnection between the parallel path flows allows correction of any potential flow misbalance which can be due, among others, to the design of the reactant passage 26 (especially the manifold design) and/or the tolerance of the manufacture process and/or plugging of a flow path.
The fluid flow rate can therefore be balanced between all the flow paths 52 of the parallel multiple flow path configuration 50.
Moreover, having the communicating zones 54 in the same volume 24 as that of the reactant passage 26 or the chamber 34, i.e. having the communicating zones 54 in the same plane as that of the parallel flow paths 52, brings some meaningful advantages: such a configuration is simple to manufacture (same plate), optimizes the thermal transfer with the thermal control passages of the volumes 12 and 14 placed on both sides of the volume 24 and avoid additional pressure drop and dead zones that are detrimental for an even Residence Time distribution and safety
According to the invention, the design of manifold 56 placed upstream of each parallel multiple flow path configuration 50 and the strict similarity of the chambers 34 and of the parallel fluid flows 52 are therefore less critical.
The two channels or flow paths 52 are adjusted in such a way that they are regularly in contact at their edges with an opening (communicating zone 54) between them being adjusted to allow a modification of flow repartition in case of different pressure drop between parallel fluid flows 52 (manufacturing tolerances or plugging for example), and small enough not to modify significantly the flow pattern at the said contact points.
The successive chambers 34 make up a significant portion of the reactant passage 26 of the embodiment of a microfluidic device represented in
For devices in which heat exchange and residence time is to be maximized, it is desirable that the multiple successive chambers 34 extend along at least 30%, preferably at least 50% of the total volume of the reactant passage 26, more desirably at least 75% or more, as is the case in the embodiment of
As may also be seen in the embodiment of the present invention in
In the variant of
In this configuration, the four adjacent chambers 34 in fluid communication with each other, each of which is part of a different path flows 52, form together a multiple flow path elementary design pattern 57 in which the fluid flows at a same level in the four parallel path flows 52.
As may be seen in the enlarged partial view of
The key advantage of multiple flow paths approach according to this invention is to reduce significantly pressure drop for a given flow rate. As an example, for an elementary design pattern formed by chambers 34 as shown on
Another way to highlight a key benefit of this multiple flow path approach is to look at maximum working flow rate corresponding to the same pressure drop. The data of
Therefore, multiple flow paths architecture according to this invention allowing a significant pressure drop reduction, it is an efficient way to increase chemical production throughput without increasing energy consumption to pump the fluids, and to keep pressure drop below typical design pressure of equipments and/or the complexity of the system through external numbering up.
Moreover, another key advantage of this high throughput design approach is to significantly reduce pressure drop (at a given flowrate) without any negative impact on pressure resistance and mixing/dispersions quality. So no compromise is needed, especially regarding:
Pressure resistance: a parallel multiple flow path configuration 50 is formed by implementing in parallel channels formed by a series of elementary design patterns (for instance chamber 34 with a heart shape of
Dispersions (or mixing) quality: as the base elementary design pattern is conserved, the efficiency of mixing is comparable to the prior art single channel designs. In case of emulsions, the quality of emulsion has been assessed using solvent & diol non-miscible liquid system. The emulsion is created in the microstructures and the fluid flowing out of the microstructure collected. Time needed for decantation was taken as a measure of the quality of the emulsion formed inside the microstructure (the higher the time, the better the quality). As reported in
As shown on
a is a configuration in which said communicating zones 54 are formed between all the pairs of two adjacent elementary design patterns (chambers 34) of all of said multiple flow path elementary design patterns 57 of said parallel multiple flow path configuration 50,
b shows an alternative in which said communicating zones 54 are formed only between the pairs of two adjacent elementary design patterns (chambers 34) of the first two multiple flow path elementary design patterns 57 located in the upstream part of said parallel multiple flow path configuration 50, and
c shows another alternative in which said communicating zones 54 are formed only between every other pair of two adjacent elementary design patterns (chambers 34) of all of said multiple flow path elementary design patterns 57 of said parallel multiple flow path configuration 50.
on
Referring to
In the embodiment of
In the embodiment of
The embodiments of
Referring to
The pillars 166 are structures serving as turbulence promoter or static mixer along the fluid flow path 152. In this context, the pillars could present other designs, including designs which have portions which are not parallel to the fluid flow direction in order to promote turbulence.
The open cells 134 are placed in series to form a flow path 152 and in parallel to form a multiple flow path elementary design pattern 157 which is limited by lateral vertical wall structures 28.
The two (or more) open cells 134 placed in parallel to form a multiple flow path elementary design pattern 157 can be aligned in the lateral direction (
The flow path elementary design patterns 134 are placed in series to form a parallel multiple flow path configuration 150 which is a continuous straight channel or a tortuous channel with important straight portions (
The pillars 166 are arranged such that in all transverse sections (all widths) of the parallel multiple flow path configuration 150, there is at least one pillar 166 (
The communicating zones 154 between two adjacent elementary design patterns or open cells 134 are openings or passages defined between at least two pillars 166 of each of these two adjacent elementary design patterns or open cells 134, notably two pillars 166 in alignment.
In the alternative staggered configuration of the pillars of
With these elementary design pattern of the second type in the form of an open cell 134 with pillars 166, sub passages of the flow path 152 are defined by the pillars 166, between the pillars 166 which are offset in the lateral direction, i.e. which are not in alignment along the flow path 152.
The elementary design pattern of the second type 134 is particularly dedicated for homogenous fluid residence time.
In
The variation of width allow for a better pressure resistance of the wall structures. Moreover, such a configuration allow a contact between two parallel elementary design patterns at the location of their larger width, which is a simple way to create a communicating zone only by creating an opening in this location of contact with a common wall.
The wavy chambers 234 are placed in series to form a flow path 252 and in parallel to form a multiple flow path elementary design pattern 257. The flow path elementary design patterns 257 are placed in series to form a parallel multiple flow path configuration 250.
In
In the alternative form of
In that case, the communicating zones 254 between two adjacent elementary design patterns or wavy chambers 234 are formed by an opening in the single wavy wall 228.
As shown on
The two (or more) wavy chambers 234 placed in parallel to form a multiple flow path elementary design pattern 257 can be aligned in the lateral direction (
As previously indicated, elementary design pattern of the first type or chamber 34, elementary design pattern of the second type or open cell 134 and elementary design pattern of the third type or wavy chamber cell 234 provide mixing and/or residence time, have a width which is not constant along the direction of the flow path and can be in flow interconnection with another elementary design pattern of the same type of the adjacent flow path.
Other elementary design patterns able to provide mixing and/or residence time can be used according to the parallel multiple flow path configuration described above, i.e notably with elementary design patterns which are adjacent to each other both in series and in parallel.
Preferably, the communicating zones are formed by a direct flow interconnection between two adjacent elementary design patterns of said multiple flow path elementary design pattern.
For each parallel multiple flow path configuration a manifold 56, 156, 256 is placed along said reactant passage upstream said parallel multiple flow path configuration in order to divide or fork said reactant passage 26 into so many flow paths as there are in the parallel multiple flow path configuration.
Due to flow interconnection between adjacent parallel flow paths, which allow for correction of flow misbalance between the parallel flow paths, the manifolds design can be simple and need to take into account fluids physical properties with limited accuracy.
These simple manifold designs are non chemical reaction dependant designs, with potentially some flow interconnection as well into manifold zone (
Other design are possible according to the invention, notably having other numbers of parallel flow paths in one parallel multiple flow path configuration: for instance three, five, six, eight parallel flow paths.
Preferably, said communicating zones 54, 154 and 254 have a length ranging from 0.5 to 6 mm, preferably from 1 to 5 mm and preferably from 1.5 to 3.5 mm.
Preferably, the height of the volume 24 and of the reactant passage 26, which is also the height of the elementary design patterns 34, 134, 234 and of the communicating zones 54, 154 and 254, ranges from 0.8 mm to 3 mm.
Preferably, said communicating zones 54, 154 and 254 have a ratio height/length ranging from 0.1 to 6, and preferably from 0.2 to 2.
Preferably, the width of said elementary design patterns along the flow path is ranging from 1 to 20 mm, and preferably from 3 to 15 mm
Preferably, the ratio between the width of said elementary design patterns along the flow path, at the location of the communicating zone 54, 154, 254, and the length of said communicating zones is ranging from 2 to 40, and preferably from 2 to 14.
According to the invention, when considering two adjacent parallel flow paths 52, 152, 252, there are at least two communicating zones 54, 154, 254 located somewhere between the inlet and the outlet of the parallel multiple flow path configuration 50, 150, 250.
Depending on elementary design patterns along the flow path, number of parallel paths, global implementation into available surface and manifold design, different numbers of communicating zones 54, 154, 254 may be needed to get fully uniform flow distribution. But most of the correction is usually done within the first two communicating zones 54, 154, 254.
The microfluidic devices according to the present invention are desirably made from one or more of glass, glass-ceramic, and ceramic. Processes for preparing such devices from glass sheets forming horizontal walls, with molded and consolidated frit positioned between the sheets forming vertical walls, are disclosed, for example, in U.S. Pat. No. 7,007,709, “Microfluidic Device and Manufacture Thereof,” but fabrication is not limited to this method.
The devices of the present invention may also include layers additional to those shown, if desired.
“Reactant” as used herein is shorthand for potentially any substance desirable to use within a microfluidic device. Thus “reactant” and “reactant passage” may refer to inert materials and passages used for such.
Number | Date | Country | Kind |
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08305610.0 | Sep 2008 | EP | regional |
08305711.7 | Oct 2008 | EP | regional |