EP2123349A2 - Emulsification device - Google Patents

Emulsification device Download PDF

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Publication number
EP2123349A2
EP2123349A2 EP09006861A EP09006861A EP2123349A2 EP 2123349 A2 EP2123349 A2 EP 2123349A2 EP 09006861 A EP09006861 A EP 09006861A EP 09006861 A EP09006861 A EP 09006861A EP 2123349 A2 EP2123349 A2 EP 2123349A2
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EP
European Patent Office
Prior art keywords
channel
liquid
phase
emulsification device
continuous
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP09006861A
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German (de)
French (fr)
Other versions
EP2123349A3 (en
EP2123349B1 (en
Inventor
Erika Katayama
Tetsuro Miyamoto
Yoshishige Endo
Shigenori Togashi
Mio Suzuki
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Hitachi Plant Technologies Ltd
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Hitachi Plant Technologies Ltd
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Publication of EP2123349A2 publication Critical patent/EP2123349A2/en
Publication of EP2123349A3 publication Critical patent/EP2123349A3/en
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Publication of EP2123349B1 publication Critical patent/EP2123349B1/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40Mixing liquids with liquids; Emulsifying
    • B01F23/41Emulsifying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/10Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30Injector mixers
    • B01F25/31Injector mixers in conduits or tubes through which the main component flows
    • B01F25/313Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
    • B01F25/3131Injector 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4338Mixers with a succession of converging-diverging cross-sections, i.e. undulating cross-section
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/434Mixing tubes comprising cylindrical or conical inserts provided with grooves or protrusions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/50Pipe mixers, i.e. mixers wherein the materials to be mixed flow continuously through pipes, e.g. column mixers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30Micromixers

Definitions

  • the present invention relates to an emulsification device. More particularly, the present invention relates to an emulsification device suitable for emulsification of two different liquids by uniformly dispersing one liquid as a disperse phase into the other liquid as a continuous phase, the liquid of the disperse phase being not dissolvable in the liquid of the continuous phase.
  • emulsion is generally produced by applying a shearing force to reduce droplets of one liquid to micro size and then dispersing them into the other liquid.
  • a batch method using a dispersion approach is known as a conventional method for forming emulsion.
  • This method obtains a large amount of emulsion at one time by using a mechanism for rotating and stirring water and oil in a large-sized container.
  • this process has a problem of nonuniform emulsion droplet size produced because of a nonuniform shearing force applied to the liquids, and another problem of a long production time.
  • Nonuniform emulsion droplet size causes variation in effect and performance of the process, resulting in quality degradation.
  • microfluidic chip supplies liquids in a micro channel having a width and a depth of several to hundreds of micrometers and performs emulsification in the micro channel.
  • water and oil are split into a number of flows which are arranged in alternation to increase the touch area between the liquids.
  • the number of water and oil flows is gradually decreased to utilize the liquid shearing rate produced between the liquids and the channel wall surface (refer, for example, to JP-A-2004-81924 ).
  • JP-A-2004-81924 provides a better droplet size distribution of emulsion than the batch method does, there is a certain breadth of distribution.
  • JP-A-2004-98225 produces emulsion droplets one by one, making it possible to provide a uniform droplet size having a dispersing value of 20% of below.
  • the sheath flow structure it is necessary to reduce the diameter d of a micro channel in order to reduce emulsion droplets to micro size.
  • the pressure loss increases in inverse proportion to the fourth power of the diameter d of the micro channel, thus decreasing possible flow rate.
  • An object of the present invention is to provide an emulsification device for mixing two different liquids not dissolvable in each other, wherein (1) emulsion droplets can be reduced to micro size without reducing the channel width, which may cause degraded productivity; and wherein (2) the disperse phase can be prevented from adhering to the channel wall surface, thus allowing the device to be operated for a prolonged period of time and a uniform emulsion droplet size to be obtained.
  • an emulsification device for mixing two different liquids not dissolvable in each other, wherein (1) emulsion droplets can be reduced to micro size without reducing the channel width, which may cause degraded productivity; and wherein (2) the disperse phase can be prevented from adhering to the channel wall surface, thus allowing the device to be operated for a prolonged period of time and a uniform emulsion droplet size to be obtained.
  • Fig. 1 shows the configuration of the system including the emulsification device according to the first embodiment of the present invention.
  • the system includes a raw material tank 101A which pools water, and a raw material tank 101B which pools oil.
  • the water pooled in the raw material tank 101A is transferred to an emulsification device 104 by a pump 102A.
  • the oil pooled in the raw material tank 101B is transferred to the emulsification device 104 by a pump 102B.
  • the two liquids transferred by the pumps 102A and 102B flow into the emulsification device 104 through introductory tubes 103A and 103B, respectively, and emulsion is produced in the emulsification device 104.
  • the produced emulsion is pooled in an emulsion tank 106 through an introductory tube 105.
  • emulsification device 104 When temperature control is required in emulsion production, it is possible, for example, to install the emulsification device 104 in a temperature-controlled bath 107 and fill the temperature-controlled bath 107 with a heating medium to perform temperature control. Alternatively, it is also possible to install a peltier device outside the emulsification device 104.
  • Figs. 2 and 3 are exploded perspective views showing the configuration of the emulsification device according to the first embodiment of the present invention.
  • Fig. 2 shows an exploded structure of the emulsification device 104 when viewed from the side of the continuous- and disperse-phase introductory members.
  • Fig. 3 shows an exploded structure of the emulsification device 104 when viewed from the side of an emulsion discharge member.
  • Figs. 4A and 4B are enlarged views of essential parts showing the configuration of the emulsification device according to the first embodiment of the present invention.
  • Fig. 4A is an enlarged plan view of an area enclosed by a broken-line circle B in Fig. 2 when viewed from the side of the liquid introductory member.
  • Fig. 4B is an enlarged perspective view of the area enclosed by the broken-line circle B in Fig. 2 when viewed from the side of the liquid introductory member.
  • Fig. 5 is a cross-sectional view showing the configuration of the emulsification device according to the first embodiment of the present invention.
  • Fig. 5 shows a cross section which passes through the center of the emulsification device, in parallel with the direction of the disperse phase flow.
  • Fig. 6 shows emulsification performed by the emulsification device according to the first embodiment of the present invention.
  • the emulsification device 104 comprises a liquid introductory member 201, a joining channel member 202, a mixing channel member 203, and a liquid discharge member 204.
  • the liquid introductory member 201 is provided with four through screw holes 205 formed at its four corners. Further, each of the joining channel member 202, the mixing channel member 203, and the liquid discharge member 204 is also provided with four screw holes formed at the same positions as the screw holes 205 of the liquid introductory member 201.
  • the liquid discharge member 204 has two registration-pin blind holes 213 formed thereon. As shown in Fig.
  • the liquid introductory member 201 is also provided with two registration-pin blind holes formed at the same positions as the registration-pin blind holes 213 of the liquid discharge member 204. Therefore, precise positioning can be achieved by inserting a registration pin (not shown) into each of the registration-pin blind holes 213. All the members can be fastened using screws (not shown) which pass through the screw holes 205.
  • Fig. 5 shows a state where the liquid introductory member 201, the joining channel member 202, the mixing channel member 203, and the liquid discharge member 204 shown in Figs. 2 and 3 are fastened with screws (not shown).
  • the liquid discharge member 204 is provided with a seal slot 206A formed around an emulsion discharge channel 212.
  • the liquid introductory member 201 is provided with a seal slot 206B formed around a continuous-phase inlet channel 301, and a seal slot 206C formed around a disperse-phase inlet channel 302.
  • the joining channel member 202 is provided with a seal slot 206D formed around a continuous-phase branching channel 303. Padding each of the seal slots 206 with a seal material (not shown) makes it possible to improve the adhesion between the members, thus preventing leak of liquid. It is also possible to bond or joint the members as required.
  • each member constituting the emulsification device 104 Metal, resin, glass, etc. are used as the material of each member constituting the emulsification device 104, according to the type of liquids to be transferred therein. Further, it is not necessary that all the members are made of the same material but each member may be made of a different material depending on the characteristics of processing, thermal conductivity, and the like.
  • a continuous-phase inlet port 207 of the liquid introductory member 201 shown in Fig. 2 communicates with the continuous-phase inlet channel 301 of the liquid introductory member 201 shown in Fig. 3 .
  • a disperse-phase inlet port 208 of the liquid introductory member 201 shown in Fig. 2 communicates with the disperse-phase inlet channel 302 of the liquid introductory member 201 shown in Fig. 3 .
  • a continuous-phase vertical channel 209 of the joining channel member 202 shown in Fig. 2 communicates with the continuous-phase branching channel 303 of the joining channel member 202 shown in Fig. 3 .
  • the continuous-phase branching channel 303 is composed of a straight portion and, in the vicinity of a disperse-phase vertical channel 210, a bifurcated channel.
  • the continuous-phase vertical channel 209 of the joining channel member 202 shown in Fig. 2 communicates with an end of the straight portion of the continuous-phase branching channel 303.
  • the disperse-phase vertical channel 210 of the joining channel member 202 shown in Fig. 2 communicates with the disperse-phase vertical channel 210 of the joining channel member 202 shown in Fig. 3 .
  • a continuous-phase horizontal channel 211 of the mixing channel member 203 shown in Fig. 2 communicates with the mixing channel 304 of the mixing channel member 203 shown in Fig. 3 .
  • the detailed configuration of the continuous-phase horizontal channel 211 will be mentioned later with reference to Fig. 4 .
  • the emulsion discharge channel 212 of the liquid discharge member 204 shown in Fig. 2 communicates with an emulsion outlet port 305 of the liquid discharge member 204 shown in Fig. 3 .
  • the continuous-phase horizontal channel 211 of the mixing channel member 203 is composed of continuous-phase horizontal channels 211A and 211B and a swirl channel 211Z having a cylindrical shape.
  • the continuous-phase horizontal channel 211A is arranged with an offset in one direction from the central axis of the swirl channel 211Z.
  • the continuous-phase horizontal channel 211B is arranged with an offset in the other direction therefrom.
  • the continuous-phase horizontal channels 211A and 211B are arranged with an offset axisymmetrically with respect to the swirl channel 211Z.
  • One channel of the bifurcated channel of the continuous-phase branching channel 303 shown in Fig. 3 is connected to an end of the continuous-phase horizontal channel 211A to form a flow toward the swirl channel 211Z.
  • the other channel of the bifurcated channel of the continuous-phase branching channel 303 shown in Fig. 3 is connected to an end of the continuous-phase horizontal channel 211B to form another flow toward the swirl channel 211Z.
  • the flow from an end of the continuous-phase horizontal channel 211A toward the swirl channel 211Z and the flow from an end of the continuous-phase horizontal channel 211B toward the swirl channel 211Z join at the swirl channel 211Z to form swirl flows.
  • the disperse-phase vertical channel 210 is arranged so that its central axis coincides with the central axis of the swirl channel 211Z.
  • the mixing channel 304 is arranged so that its central axis coincides with the central axis of the swirl channel 211Z.
  • the water to be used as a continuous phase and the oil to be used as a disperse phase are introduced from the continuous-phase inlet port 207 and the disperse-phase inlet port 208, respectively, into the liquid introductory member 201.
  • the introductory tubes 103A and 103B shown in Fig. 1 are connected to the continuous-phase inlet port 207 and the disperse-phase inlet port 208, respectively, by using a joint (not shown) so as to transfer the liquids into the emulsification device 104 through the pumps 102A and 102B, respectively.
  • the water introduced from continuous-phase inlet port 207 into the emulsification device 104 passes through the continuous-phase inlet channel 301 and the continuous-phase vertical channel 209. After being distributed by the continuous-phase branching channel 303, the water flows into the mixing channel 304. The continuous phase is swirled in the mixing channel 304.
  • the oil introduced from the disperse-phase inlet port 208 passes through the disperse-phase inlet channel 302 and the disperse-phase vertical channel 210 formed so as to be perpendicular to a laminar plane of the liquid introductory member 201. Then, the oil flows into a joining point of the mixing channel 304. The two liquids join at the joining point.
  • Fig. 6 shows the behavior of the two liquids at the joining point.
  • the water and oil join in the mixing channel 304 the water wraps around the oil to form swirl flows 401.
  • an emulsion droplet 601 is stably formed.
  • the formed emulsion droplet 601 passes through the emulsion discharge channel 212, the emulsion outlet port 305, and the introductory tube 105, and then is pooled in the emulsion tank 106.
  • each channel is not limited to the one shown in the present embodiment but may be, for example, rectangular.
  • the water pooled in the raw material tank 101A contains surfactant, and the oil pooled in the raw material tank 101B is silicon oil.
  • Fig. 10 shows results of an experiment which includes two different cases.
  • the central axes of the continuous-phase horizontal channels 211A and 211B are arranged so as to intersect with the central axis of a swirl portion so that a swirl component of the continuous phase is not provided (therefore, swirl flows are not formed; not shown).
  • the central axes of the continuous-phase horizontal channels 211A and 211B are arranged with an offset from the central axis of the swirl portion (therefore, swirl flows are formed).
  • Fig. 10 shows results of the experiment performed under five liquid transfer conditions (case1 to case5). The results are arranged in ascending order of the total flow rate of the continuous and disperse phases transferred.
  • the average emulsion droplet size in the emulsion produced when swirl flows are formed is about 10% smaller than that in the emulsion produced when swirl flows are not formed. Further, the average dispersion value when swirl flows are formed is almost the same as that when swirl flows are not formed (the difference is less than 10%). We confirmed that variation in droplet size is small.
  • Fig. 7 is a perspective view showing another configuration of the emulsion discharge channel in the emulsification device according to the first embodiment of the present invention.
  • the same reference numerals as in Fig. 4 denote identical parts.
  • the configuration according to the present embodiment includes continuous-phase horizontal channels 211C and 211D in addition to the continuous-phase horizontal channels 211A and 211B, and the swirl channel 211Z having a cylindrical shape shown in Fig. 4 .
  • the continuous-phase horizontal channels 211C and 211D are also arranged with an offset from the central axis of the swirl channel 211Z.
  • the continuous-phase horizontal channels 211A, 211B, 211C, and 211D are arranged with an offset axisymmetrically with respect to the swirl channel 211Z, each being positioned at intervals of 90 degrees.
  • the four continuous phases flowing in from four directions increase the swirling force of the continuous phases. Further, since a shearing force is equally applied from four directions, the liquid droplet formation can be stabilized in comparison with the case of Fig. 4 where continuous phases flow in from two directions.
  • disperse-phase vertical channel 210 and the mixing channel 304 are arranged so that their central axes coincide with the central axis of the swirl channel 211Z, it is only necessary that the central axis of the disperse-phase vertical channel 210 approximately coincide with the central axis of the mixing channel 304. For example, it is only necessary that the central axis of the disperse-phase vertical channel 210 be located within a cross section of the mixing channel 304.
  • the continuous phases give a swirl effect to the shearing force, relatively increasing the force applied to the boundary surface between the continuous and disperse phases in comparison with a laminar flow state. Accordingly, emulsion droplets can be reduced to micro size without reducing the channel width. In other words, in order to obtain emulsion droplets having the same droplet size, the channel width can be made larger than that in conventional cases and therefore the productivity can be improved. Further, wrapping around the disperse phase with continuous phases makes it possible to prevent the disperse phase from adhering to the channel wall surface, which may cause variation in droplet size, thus allowing uniform emulsification for a prolonged period of time even without cleaning.
  • the configuration of the emulsification device according to a second embodiment of the present invention will be explained below with reference to Fig. 8 .
  • the configuration of a system including the emulsification device according to the present embodiment is the same as that shown in Fig. 1 . Further, the configuration of the emulsification device according to the present embodiment is the same as that shown in Figs. 2 and 3 .
  • Fig. 8 is an enlarged perspective view of essential parts showing the configuration of the emulsification device according to the second embodiment of the present invention.
  • FIG. 8 An example shown in Fig. 8 is a modified version of the mixing channel member 203 of the example shown in Figs. 2 and 4 .
  • the mixing channel 304 in Fig. 8 has a spiral convex portion 801 formed on the channel wall surface.
  • the spiral convex portion 801 is formed like an internal thread.
  • the swirl channel 211 is connected to the mixing channel 304 from the direction which perpendicularly intersects with the central axis of the mixing channel 304. Further, the disperse-phase vertical channel 210 is connected to the mixing channel 304 so that its central axis coincides with the central axis of the mixing channel 304.
  • This configuration allows the continuous phase supplied from the swirl channel 211 to form spiral flows 401 in the outer circumference of the disperse phase supplied from the disperse-phase vertical channel 210 and to swirl them.
  • the continuous phase gives a swirl effect to the shearing force, making it possible to reduce emulsion droplets to micro size without reducing the channel width.
  • the channel width can be made larger than that in conventional cases and therefore the productivity can be improved.
  • wrapping around the disperse phase with continuous phases makes it possible to prevent the disperse phase from adhering to the channel wall surface, which may cause variation in droplet size, thus allowing uniform emulsification for a prolonged period of time even without cleaning.
  • the configuration of an emulsification device according to a third embodiment of the present invention will be explained below with reference to Fig. 9 .
  • the configuration of a system including the emulsification device according to the present embodiment is the same as that shown in Fig. 1 . Further, the configuration of the emulsification device according to the present embodiment is the same as that shown in Figs. 2 and 3 .
  • Fig. 9 is an enlarged perspective view of essential parts showing the configuration of the emulsification device according to the third embodiment of the present invention.
  • FIG. 8 An example shown in Fig. 8 is a modified version of the mixing channel member 203 of the example shown in Figs. 2 and 4 .
  • an example shown in Fig. 9 generates a swirl flow by using external energy.
  • the upstream side of the mixing channel 304 has a double-pipe structure with which a vertical channel 901 of the continuous-phase mixing channel member is arranged on the outer side and the disperse-phase vertical channel 210 on the inner side.
  • the vertical channel 901 of the continuous-phase mixing channel member is provided with a rotor 902.
  • a rotating mechanism 903 rotates the rotor 902
  • the continuous phase flowing in the vertical channel 901 of the continuous-phase mixing channel member receives a swirling force, thus allowing the continuous phase to flow into the mixing channel 304 while forming a swirl flow.
  • the continuous phase gives a swirl effect to the shearing force, making it possible to reduce emulsion droplets to micro size without reducing the channel width.
  • the channel width can be made larger than that in conventional cases and therefore the productivity can be improved.
  • wrapping around the disperse phase with the continuous phases makes it possible to prevent the disperse phase from adhering to the channel wall surface, which may cause variation in droplet size, thus allowing uniform emulsification for a prolonged period of time even without cleaning.

Abstract

There is provided an emulsification device for mixing two different liquids not dissolvable in each other, wherein (1) emulsion droplets can be reduced to micro size without reducing the channel width, which may cause degraded productivity; and wherein (2) a disperse phase can be prevented from adhering to the channel wall surface, thus allowing the device to be operated for a prolonged period of time and a uniform emulsion droplet size to be obtained.
The emulsification device comprises: at least one channel (211) of a first liquid; a channel (210) of a second liquid; and a mixing channel (304) in which the first liquid is joined with the second liquid. In the mixing channel (304), the first liquid has a swirl component in the mainstream direction. The channel of the second liquid is connected to the central portion of the mixing channel, and the second liquid flows at the central portion of at least one swirl flow of the first liquid. In this way, at least one continuous-phase swirl flow is formed around the disperse phase.

Description

    BACKGROUND OF THE INVENTION 1. Field of the Invention
  • The present invention relates to an emulsification device. More particularly, the present invention relates to an emulsification device suitable for emulsification of two different liquids by uniformly dispersing one liquid as a disperse phase into the other liquid as a continuous phase, the liquid of the disperse phase being not dissolvable in the liquid of the continuous phase.
  • 2. Description of the Related Art
  • With two different liquids not dissolvable in each other, such as water and oil, emulsion is generally produced by applying a shearing force to reduce droplets of one liquid to micro size and then dispersing them into the other liquid.
  • A batch method using a dispersion approach is known as a conventional method for forming emulsion. This method obtains a large amount of emulsion at one time by using a mechanism for rotating and stirring water and oil in a large-sized container. However, this process has a problem of nonuniform emulsion droplet size produced because of a nonuniform shearing force applied to the liquids, and another problem of a long production time. Nonuniform emulsion droplet size causes variation in effect and performance of the process, resulting in quality degradation.
  • To solve the above-mentioned problems, emulsion production by using a microfluidic chip has been advocated in recent years. The microfluidic chip supplies liquids in a micro channel having a width and a depth of several to hundreds of micrometers and performs emulsification in the micro channel.
  • Specifically, with a known method for producing emulsion, water and oil are split into a number of flows which are arranged in alternation to increase the touch area between the liquids. The number of water and oil flows is gradually decreased to utilize the liquid shearing rate produced between the liquids and the channel wall surface (refer, for example, to JP-A-2004-81924 ).
  • Further, there is another known method for producing emulsion by forming a laminar sheath flow having a disperse phase as an inner laminar flow and continuous phases as outer laminar flows. With this method, the liquid transfer rate of the continuous phases is controlled to apply a shearing force to the boundary surface between the continuous and disperse phases. Then, the pressure is rapidly reduced by a suddenly expanded portion provided immediately after the portion where the shearing force is applied, thus segmentalizing the disperse phase into droplets (refer, for example, to JP-A-2004-98225 ).
  • SUMMARY OF THE INVENTION
  • Although the emulsification method disclosed in JP-A-2004-81924 provides a better droplet size distribution of emulsion than the batch method does, there is a certain breadth of distribution.
  • On the other hand, the method described in JP-A-2004-98225 produces emulsion droplets one by one, making it possible to provide a uniform droplet size having a dispersing value of 20% of below. However, with the sheath flow structure, it is necessary to reduce the diameter d of a micro channel in order to reduce emulsion droplets to micro size. However, there has been a problem that, with reduced channel width, the pressure loss increases in inverse proportion to the fourth power of the diameter d of the micro channel, thus decreasing possible flow rate. With the sheath flow structure described in JP-A-2004-98225 , although the disperse phase does not come in direct contact with the channel since the continuous phases flow outside the disperse phase in two directions in which the continuous phases flow, the disperse phase comes in direct contact with the channel in the other two directions. It has been found that the disperse phase adheres to the inner wall surface of the channel after use for a prolonged period of time possibly resulting in variation in droplet size.
  • An object of the present invention is to provide an emulsification device for mixing two different liquids not dissolvable in each other, wherein (1) emulsion droplets can be reduced to micro size without reducing the channel width, which may cause degraded productivity; and wherein (2) the disperse phase can be prevented from adhering to the channel wall surface, thus allowing the device to be operated for a prolonged period of time and a uniform emulsion droplet size to be obtained.
    1. (1) In order to attain the above-mentioned object, the present invention provides an emulsification device for mixing and emulsifying two different liquids not dissolvable in each other, comprising: a channel of a first liquid; a channel of a second liquid; and a mixing channel in which the first liquid is joined with the second liquid; wherein the first liquid has a swirl component in the mainstream direction in the mixing channel; and wherein the channel of the second liquid is connected to the central portion of the mixing channel, and the second liquid flows at the central portion of a swirl flow of the first liquid.
      This configuration of the emulsification device for mixing two different liquids not dissolvable in each other makes it possible to reduce emulsion droplets to micro size without reducing the channel width, which may cause degraded productivity, and to prevent the disperse phase from adhering to the channel wall surface, thus allowing the device to be operated for a prolonged period of time and uniform emulsion droplet to be obtained.
    2. (2) The emulsification device according to (1) above, wherein, preferably, the central axis of the channel of the first liquid is arranged with an offset from the central axis of the mixing channel.
    3. (3) The emulsification device according to (2) above, wherein, preferably, a plurality of channels of the first liquid are provided, each of the plurality of channels of the first liquid being arranged axisymmetrically with respect to the central axis of the mixing channel.
    4. (4) The emulsification device according to (1) above, wherein, preferably, the central axis of the channel of the second liquid is arranged in a projection plane of the mixing channel.
    5. (5) The emulsification device according to (1) above, wherein, preferably, the mixing channel is provided with a spiral convex portion on its wall surface to generate a swirling force in the first liquid.
    6. (6) The emulsification device according to (1) above, wherein, preferably, the channel of the first liquid is arranged around the channel of the second liquid in double-pipe form; wherein a rotor is provided in the channel of the first liquid; and wherein the emulsification device is provided with a rotating mechanism for driving the rotor.
  • In accordance with the present invention, there is provided an emulsification device for mixing two different liquids not dissolvable in each other, wherein (1) emulsion droplets can be reduced to micro size without reducing the channel width, which may cause degraded productivity; and wherein (2) the disperse phase can be prevented from adhering to the channel wall surface, thus allowing the device to be operated for a prolonged period of time and a uniform emulsion droplet size to be obtained.
  • BRIEF DESCRIPTION OF THE DRAWINGS
    • Fig. 1 shows the configuration of a system including an emulsification device according to a first embodiment of the present invention.
    • Fig. 2 is an exploded perspective view showing the configuration of the emulsification device according to the first embodiment of the present invention.
    • Fig. 3 is an exploded perspective view showing the configuration of the emulsification device according to the first embodiment of the present invention.
    • Figs. 4A and 4B are enlarged views of essential parts showing the configuration of the emulsification device according to the first embodiment of the present invention.
    • Fig. 5 is a cross-sectional view showing the configuration of the emulsification device according to the first embodiment of the present invention.
    • Fig. 6 shows the emulsification in the emulsification device according to the first embodiment of the present invention.
    • Fig. 7 is a perspective view showing another configuration of an emulsion discharge channel in the emulsification device according to the first embodiment of the present invention.
    • Fig. 8 is an enlarged perspective view of essential parts showing the configuration of an emulsification device according to a second embodiment of the present invention.
    • Fig. 9 is an enlarged perspective view of essential parts showing the configuration of an emulsification device according to a third embodiment of the present invention.
    • Fig. 10 shows results of experiment in a case where a continuous phase is swirled and a case where it is not under the same liquid transfer conditions when the emulsification device according to the first embodiment of the present invention is used.
    DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
  • The configuration and operations of an emulsification device according to a first embodiment of the present invention will be explained below with reference to Figs. 1 to 7.
  • First of all, the configuration of a system including the emulsification device according to the present embodiment will be explained below with reference to Fig. 1.
  • Fig. 1 shows the configuration of the system including the emulsification device according to the first embodiment of the present invention.
  • The system includes a raw material tank 101A which pools water, and a raw material tank 101B which pools oil. The water pooled in the raw material tank 101A is transferred to an emulsification device 104 by a pump 102A. The oil pooled in the raw material tank 101B is transferred to the emulsification device 104 by a pump 102B. Here, it is desirable to properly use a syringe pump or a gear pump as the pumps 102A and 102B depending on the object.
  • The two liquids transferred by the pumps 102A and 102B flow into the emulsification device 104 through introductory tubes 103A and 103B, respectively, and emulsion is produced in the emulsification device 104. The produced emulsion is pooled in an emulsion tank 106 through an introductory tube 105.
  • When temperature control is required in emulsion production, it is possible, for example, to install the emulsification device 104 in a temperature-controlled bath 107 and fill the temperature-controlled bath 107 with a heating medium to perform temperature control. Alternatively, it is also possible to install a peltier device outside the emulsification device 104.
  • The configuration of the emulsification device according to the present embodiment is explained below with reference to Figs. 2 to 6.
  • Figs. 2 and 3 are exploded perspective views showing the configuration of the emulsification device according to the first embodiment of the present invention. Fig. 2 shows an exploded structure of the emulsification device 104 when viewed from the side of the continuous- and disperse-phase introductory members. Fig. 3 shows an exploded structure of the emulsification device 104 when viewed from the side of an emulsion discharge member.
  • Figs. 4A and 4B are enlarged views of essential parts showing the configuration of the emulsification device according to the first embodiment of the present invention. Fig. 4A is an enlarged plan view of an area enclosed by a broken-line circle B in Fig. 2 when viewed from the side of the liquid introductory member. Fig. 4B is an enlarged perspective view of the area enclosed by the broken-line circle B in Fig. 2 when viewed from the side of the liquid introductory member. Fig. 5 is a cross-sectional view showing the configuration of the emulsification device according to the first embodiment of the present invention. Fig. 5 shows a cross section which passes through the center of the emulsification device, in parallel with the direction of the disperse phase flow. Fig. 6 shows emulsification performed by the emulsification device according to the first embodiment of the present invention.
  • As shown in Figs. 2 and 3, the emulsification device 104 comprises a liquid introductory member 201, a joining channel member 202, a mixing channel member 203, and a liquid discharge member 204. The liquid introductory member 201 is provided with four through screw holes 205 formed at its four corners. Further, each of the joining channel member 202, the mixing channel member 203, and the liquid discharge member 204 is also provided with four screw holes formed at the same positions as the screw holes 205 of the liquid introductory member 201. The liquid discharge member 204 has two registration-pin blind holes 213 formed thereon. As shown in Fig. 3, the liquid introductory member 201 is also provided with two registration-pin blind holes formed at the same positions as the registration-pin blind holes 213 of the liquid discharge member 204. Therefore, precise positioning can be achieved by inserting a registration pin (not shown) into each of the registration-pin blind holes 213. All the members can be fastened using screws (not shown) which pass through the screw holes 205. Fig. 5 shows a state where the liquid introductory member 201, the joining channel member 202, the mixing channel member 203, and the liquid discharge member 204 shown in Figs. 2 and 3 are fastened with screws (not shown).
  • As shown in Fig. 2, the liquid discharge member 204 is provided with a seal slot 206A formed around an emulsion discharge channel 212. As shown in Fig. 3, the liquid introductory member 201 is provided with a seal slot 206B formed around a continuous-phase inlet channel 301, and a seal slot 206C formed around a disperse-phase inlet channel 302. Further, the joining channel member 202 is provided with a seal slot 206D formed around a continuous-phase branching channel 303. Padding each of the seal slots 206 with a seal material (not shown) makes it possible to improve the adhesion between the members, thus preventing leak of liquid. It is also possible to bond or joint the members as required.
  • Metal, resin, glass, etc. are used as the material of each member constituting the emulsification device 104, according to the type of liquids to be transferred therein. Further, it is not necessary that all the members are made of the same material but each member may be made of a different material depending on the characteristics of processing, thermal conductivity, and the like.
  • A continuous-phase inlet port 207 of the liquid introductory member 201 shown in Fig. 2 communicates with the continuous-phase inlet channel 301 of the liquid introductory member 201 shown in Fig. 3. A disperse-phase inlet port 208 of the liquid introductory member 201 shown in Fig. 2 communicates with the disperse-phase inlet channel 302 of the liquid introductory member 201 shown in Fig. 3.
  • A continuous-phase vertical channel 209 of the joining channel member 202 shown in Fig. 2 communicates with the continuous-phase branching channel 303 of the joining channel member 202 shown in Fig. 3. The continuous-phase branching channel 303 is composed of a straight portion and, in the vicinity of a disperse-phase vertical channel 210, a bifurcated channel. The continuous-phase vertical channel 209 of the joining channel member 202 shown in Fig. 2 communicates with an end of the straight portion of the continuous-phase branching channel 303. The disperse-phase vertical channel 210 of the joining channel member 202 shown in Fig. 2 communicates with the disperse-phase vertical channel 210 of the joining channel member 202 shown in Fig. 3.
  • A continuous-phase horizontal channel 211 of the mixing channel member 203 shown in Fig. 2 communicates with the mixing channel 304 of the mixing channel member 203 shown in Fig. 3. The detailed configuration of the continuous-phase horizontal channel 211 will be mentioned later with reference to Fig. 4.
  • The emulsion discharge channel 212 of the liquid discharge member 204 shown in Fig. 2 communicates with an emulsion outlet port 305 of the liquid discharge member 204 shown in Fig. 3.
  • As shown in Fig. 4A, the continuous-phase horizontal channel 211 of the mixing channel member 203 is composed of continuous-phase horizontal channels 211A and 211B and a swirl channel 211Z having a cylindrical shape. The continuous-phase horizontal channel 211A is arranged with an offset in one direction from the central axis of the swirl channel 211Z. The continuous-phase horizontal channel 211B is arranged with an offset in the other direction therefrom. In other words, the continuous-phase horizontal channels 211A and 211B are arranged with an offset axisymmetrically with respect to the swirl channel 211Z.
  • One channel of the bifurcated channel of the continuous-phase branching channel 303 shown in Fig. 3 is connected to an end of the continuous-phase horizontal channel 211A to form a flow toward the swirl channel 211Z. The other channel of the bifurcated channel of the continuous-phase branching channel 303 shown in Fig. 3 is connected to an end of the continuous-phase horizontal channel 211B to form another flow toward the swirl channel 211Z. The flow from an end of the continuous-phase horizontal channel 211A toward the swirl channel 211Z and the flow from an end of the continuous-phase horizontal channel 211B toward the swirl channel 211Z join at the swirl channel 211Z to form swirl flows.
  • As shown in Fig. 4B, the disperse-phase vertical channel 210 is arranged so that its central axis coincides with the central axis of the swirl channel 211Z. Likewise, the mixing channel 304 is arranged so that its central axis coincides with the central axis of the swirl channel 211Z.
  • The overall liquid flows in the emulsification device 104 will be explained below with reference to Fig. 5.
  • The water to be used as a continuous phase and the oil to be used as a disperse phase are introduced from the continuous-phase inlet port 207 and the disperse-phase inlet port 208, respectively, into the liquid introductory member 201. The introductory tubes 103A and 103B shown in Fig. 1 are connected to the continuous-phase inlet port 207 and the disperse-phase inlet port 208, respectively, by using a joint (not shown) so as to transfer the liquids into the emulsification device 104 through the pumps 102A and 102B, respectively.
  • The water introduced from continuous-phase inlet port 207 into the emulsification device 104 passes through the continuous-phase inlet channel 301 and the continuous-phase vertical channel 209. After being distributed by the continuous-phase branching channel 303, the water flows into the mixing channel 304. The continuous phase is swirled in the mixing channel 304.
  • On the other hand, the oil introduced from the disperse-phase inlet port 208 passes through the disperse-phase inlet channel 302 and the disperse-phase vertical channel 210 formed so as to be perpendicular to a laminar plane of the liquid introductory member 201. Then, the oil flows into a joining point of the mixing channel 304. The two liquids join at the joining point.
  • Fig. 6 shows the behavior of the two liquids at the joining point. When the water and oil join in the mixing channel 304, the water wraps around the oil to form swirl flows 401. As a result, an emulsion droplet 601 is stably formed.
  • The formed emulsion droplet 601 passes through the emulsion discharge channel 212, the emulsion outlet port 305, and the introductory tube 105, and then is pooled in the emulsion tank 106.
  • Here, the shape of each channel is not limited to the one shown in the present embodiment but may be, for example, rectangular.
  • An embodiment according to the present invention will be concretely explained below.
  • With the present embodiment, the water pooled in the raw material tank 101A contains surfactant, and the oil pooled in the raw material tank 101B is silicon oil.
  • Fig. 10 shows results of an experiment which includes two different cases. In one case, the central axes of the continuous-phase horizontal channels 211A and 211B are arranged so as to intersect with the central axis of a swirl portion so that a swirl component of the continuous phase is not provided (therefore, swirl flows are not formed; not shown). In the other case, the central axes of the continuous-phase horizontal channels 211A and 211B are arranged with an offset from the central axis of the swirl portion (therefore, swirl flows are formed). In the experiment, we used different flow rates of the water flowing in the continuous-phase horizontal channels 211A and 211B and different flow rates of the silicon oil flowing in the liquid introductory member 201, and compared results obtained under five different liquid transfer conditions. Fig. 10 shows results of the experiment performed under five liquid transfer conditions (case1 to case5). The results are arranged in ascending order of the total flow rate of the continuous and disperse phases transferred.
  • When the emulsification device is operated under the above-mentioned five different conditions, the average emulsion droplet size in the emulsion produced when swirl flows are formed is about 10% smaller than that in the emulsion produced when swirl flows are not formed. Further, the average dispersion value when swirl flows are formed is almost the same as that when swirl flows are not formed (the difference is less than 10%). We confirmed that variation in droplet size is small.
  • Another configuration of the emulsion discharge channel in the emulsification device according to the present embodiment will be explained below with reference to Fig. 7.
  • Fig. 7 is a perspective view showing another configuration of the emulsion discharge channel in the emulsification device according to the first embodiment of the present invention. The same reference numerals as in Fig. 4 denote identical parts.
  • In this example, four continuous-phase horizontal channels 211A, 211B, 211C, and 211D are arranged around the disperse-phase inlet channel 210. This configuration allows continuous phases to flow in from four directions. Specifically, the configuration according to the present embodiment includes continuous-phase horizontal channels 211C and 211D in addition to the continuous-phase horizontal channels 211A and 211B, and the swirl channel 211Z having a cylindrical shape shown in Fig. 4. The continuous-phase horizontal channels 211C and 211D are also arranged with an offset from the central axis of the swirl channel 211Z. In other words, the continuous-phase horizontal channels 211A, 211B, 211C, and 211D are arranged with an offset axisymmetrically with respect to the swirl channel 211Z, each being positioned at intervals of 90 degrees.
  • In this example, the four continuous phases flowing in from four directions increase the swirling force of the continuous phases. Further, since a shearing force is equally applied from four directions, the liquid droplet formation can be stabilized in comparison with the case of Fig. 4 where continuous phases flow in from two directions.
  • In the example shown in Fig. 4B, although the disperse-phase vertical channel 210 and the mixing channel 304 are arranged so that their central axes coincide with the central axis of the swirl channel 211Z, it is only necessary that the central axis of the disperse-phase vertical channel 210 approximately coincide with the central axis of the mixing channel 304. For example, it is only necessary that the central axis of the disperse-phase vertical channel 210 be located within a cross section of the mixing channel 304.
  • In accordance with the present embodiment, as explained above, the continuous phases give a swirl effect to the shearing force, relatively increasing the force applied to the boundary surface between the continuous and disperse phases in comparison with a laminar flow state. Accordingly, emulsion droplets can be reduced to micro size without reducing the channel width. In other words, in order to obtain emulsion droplets having the same droplet size, the channel width can be made larger than that in conventional cases and therefore the productivity can be improved. Further, wrapping around the disperse phase with continuous phases makes it possible to prevent the disperse phase from adhering to the channel wall surface, which may cause variation in droplet size, thus allowing uniform emulsification for a prolonged period of time even without cleaning.
  • The configuration of the emulsification device according to a second embodiment of the present invention will be explained below with reference to Fig. 8. The configuration of a system including the emulsification device according to the present embodiment is the same as that shown in Fig. 1. Further, the configuration of the emulsification device according to the present embodiment is the same as that shown in Figs. 2 and 3.
  • Fig. 8 is an enlarged perspective view of essential parts showing the configuration of the emulsification device according to the second embodiment of the present invention.
  • An example shown in Fig. 8 is a modified version of the mixing channel member 203 of the example shown in Figs. 2 and 4. The mixing channel 304 in Fig. 8 has a spiral convex portion 801 formed on the channel wall surface. The spiral convex portion 801 is formed like an internal thread.
  • On the inlet side of the mixing channel 304, the swirl channel 211 is connected to the mixing channel 304 from the direction which perpendicularly intersects with the central axis of the mixing channel 304. Further, the disperse-phase vertical channel 210 is connected to the mixing channel 304 so that its central axis coincides with the central axis of the mixing channel 304.
  • This configuration allows the continuous phase supplied from the swirl channel 211 to form spiral flows 401 in the outer circumference of the disperse phase supplied from the disperse-phase vertical channel 210 and to swirl them.
  • Also with the present embodiment, the continuous phase gives a swirl effect to the shearing force, making it possible to reduce emulsion droplets to micro size without reducing the channel width. In other words, in order to obtain emulsion droplets having the same droplet size, the channel width can be made larger than that in conventional cases and therefore the productivity can be improved. Further, wrapping around the disperse phase with continuous phases makes it possible to prevent the disperse phase from adhering to the channel wall surface, which may cause variation in droplet size, thus allowing uniform emulsification for a prolonged period of time even without cleaning.
  • The configuration of an emulsification device according to a third embodiment of the present invention will be explained below with reference to Fig. 9. The configuration of a system including the emulsification device according to the present embodiment is the same as that shown in Fig. 1. Further, the configuration of the emulsification device according to the present embodiment is the same as that shown in Figs. 2 and 3.
  • Fig. 9 is an enlarged perspective view of essential parts showing the configuration of the emulsification device according to the third embodiment of the present invention.
  • An example shown in Fig. 8 is a modified version of the mixing channel member 203 of the example shown in Figs. 2 and 4. On the other hand, an example shown in Fig. 9 generates a swirl flow by using external energy. Specifically, the upstream side of the mixing channel 304 has a double-pipe structure with which a vertical channel 901 of the continuous-phase mixing channel member is arranged on the outer side and the disperse-phase vertical channel 210 on the inner side. The vertical channel 901 of the continuous-phase mixing channel member is provided with a rotor 902. When a rotating mechanism 903 rotates the rotor 902, the continuous phase flowing in the vertical channel 901 of the continuous-phase mixing channel member receives a swirling force, thus allowing the continuous phase to flow into the mixing channel 304 while forming a swirl flow.
  • Also with the present embodiment, the continuous phase gives a swirl effect to the shearing force, making it possible to reduce emulsion droplets to micro size without reducing the channel width. In other words, in order to obtain emulsion droplets having the same droplet size, the channel width can be made larger than that in conventional cases and therefore the productivity can be improved. Further, wrapping around the disperse phase with the continuous phases makes it possible to prevent the disperse phase from adhering to the channel wall surface, which may cause variation in droplet size, thus allowing uniform emulsification for a prolonged period of time even without cleaning.
  • Further, the use of external energy makes it possible to reliably swirl the continuous phase without depending on the liquid transfer flow rate of the continuous phase.

Claims (6)

  1. An emulsification device for mixing and emulsifying two different liquids not dissolvable in each other, comprising:
    a channel of a first liquid;
    a channel of a second liquid; and
    a mixing channel in which the first liquid is joined with the second liquid;
    wherein, in the mixing channel, the first liquid has a swirl component in the mainstream direction; and
    wherein the channel of the second liquid is connected to the central portion of the mixing channel, and the second liquid flows at the central portion of a swirl flow of the first liquid.
  2. The emulsification device according to Claim 1,
    wherein the central axis of the channel of the first liquid is arranged with an offset from the central axis of the mixing channel.
  3. The emulsification device according to Claim 2,
    wherein a plurality of channels of the first liquid are provided; and
    wherein each of the plurality of channels of the first liquid is arranged axisymmetrically with respect to the central axis of the mixing channel.
  4. The emulsification device according to Claim 1,
    wherein the central axis of the channel of the second liquid is arranged in a projection plane of the mixing channel.
  5. The emulsification device according to Claim 1,
    wherein the mixing channel is provided with a spiral convex portion on its wall surface to generate a swirling force in the first liquid.
  6. The emulsification device according to Claim 1,
    wherein the channel of the first liquid is arranged around the channel of the second liquid in double-pipe form;
    wherein the emulsification device further comprises:
    a rotor provided in the channel of the first liquid; and
    a rotating mechanism for driving the rotor.
EP09006861A 2008-05-21 2009-05-20 Emulsification device Not-in-force EP2123349B1 (en)

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JP2009279507A (en) 2009-12-03
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CN101584972A (en) 2009-11-25
EP2123349B1 (en) 2013-01-02
JP4798174B2 (en) 2011-10-19

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