• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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    • 专利摘要:
    This invention describes a method for generating simple and compound emulsions of controllable micrometric diameters and coatings, by means of a device formed by elements of characteristic dimensions of the order of a millimeter. The generation of emulsions is obtained by the suction produced by the flow of a viscous liquid through the section of a capillary tube of millimeter size. According to a parametric determination, the liquid or the pair of liquids to be emulsified forms a simple or compound stationary capillary jet of micrometric diameter: which breaks by capillary instability forming simple or compound monadisperse microdroplets. The invention described in this specification has application in those industrial sectors in which the production of single and compound emulsions monodisperse, homogeneous and of controllable diameters and coatings of micrometric size is an essential part of the process. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2564893A1
    申请号:ES201400698
    申请日:2014-08-25
    公开日:2016-03-29
    发明作者:José Manuel Gordillo Arias de Saavedra；Álvaro EVANGELIO SÁNCHEZ；Francisco DEL CAMPO CORTÉS
    申请人:Universidad de Sevilla；
    IPC主号:
    专利说明:

    image 1 DESCRIPTION
    Procedure and device for generating simple and compound micrometric emulsions
    Object of the invention
    The invention described herein corresponds to the Scientific and Technical Area of Microfluidics. The study of microfluids is a multidisciplinary field that includes parts of Physics, Chemistry, Engineering and Biotechnology. Investigate the behavior of fluids in the microscale, where the regime of motion is laminar, gravity and inertia are negligible and viscosity and surface tension are dominant. This scientific and technical area includes the design of systems
    - devices and procedures - for the controlled production of simple and compound stationary jets that break capillary producing simple and compound drops that are used in turn for the production of fibers, tubes and capsules of micro and submicron size.
    The interest of various sectors of activity of different industries is known for the generation of simple and compound emulsions formed by micrometric-sized drops with or without coating. For example, the food industries (encapsulation of additives), phytosanitary, cosmetic, pharmaceutical (transport selective of active ingredients), chemistry (manufacture of detergents), or materials (manufacture of optical devices using liquid crystals), among others. In general. The process and the device for generating emulsions object of the invention described herein have application in those industrial sectors in which the production of simple and compound monodispersed, homogeneous emulsions and of diameters and controllable micrometer-sized coatings is an essential part of the process. . State of the art
    In recent years, studies, inventions and applications related to the microscopic control of fluid currents have multiplied, and among these studies and inventions are those that involve free surfaces or interfaces between two immiscible fluids in order to achieve microscopic structures (micro-drops , micro-bubbles, micro-capsules, etc.) in a reproducible and robust way. It is worth highlighting here two peculiar phenomena / inventions representative of the generation of micro-jets: (i) the electrospray or production of micro-jets of liquid by electrostatic forces, known for centuries, and (ii) the capillary "flow focusing", which employs pressure forces (purely mechanical) and a "focusing" hole to generate the jet. Responding to their geometry, both methods genuinely present an axial symmetry (axilsymmetric) in the area of the interface in which the jet is produced, although there are materializations of flow-focusing devices in practically two-dimensional geometries (Anna et al, Appl. Phys. Lett, (2003). 82, 364-366, Gordillo et al., Phys. Fluids, (2004), 16, 2828-2834).
    In the case of electrospray, the main drawbacks come from (i) the inherent and inevitable dependence of the phenomenon on the electrical properties of the liquid, which greatly limits the physicochemical parametric freedom of the method (although applications of enormous relevance in biochemistry have emerged - mass spectrometry of biological molecules). (ii) the small productivity of the method (very small mass flow) and the difficulty in "scaling" or "multiplying" (multiplexing) and (iii) the mediocre robustness of the method due to its great dependence on surface conditions and tube sizes of liquid feeding.
    image2
    In axilsimetric "flow focusing", although the inconveniences of dependence with respect to the electrical properties of the fluid are eliminated, there are still problems regarding the alignment of the feeding tubes with respect to the focusing holes. In 2D flow-focusing implementations, the main problem comes from wetting with the surfaces that confine the fluid to be dispersed.
    The reason why the controlled production of micro and submicron particles is one of the most active research lines within the field of Fluid Mechanics, is because of the large number of applications both scientific and technological. For example, as indicated in the article "Micro-and nanoparticles via capillary flows", Barrero and Loscertales. Annual Review of Fluid Mechanics. (2007). 39, 89-106, the efficient absorption of new drugs by tissues and organs requires that the active product be confined in droplets of substantially smaller sizes than 10 microns. Emulsions formed by micrometer-sized drops also have application in many other fields, such as the food industry. or the science of materials (manufacture of optical devices using liquid crystals), among others. At present there are a considerable number of procedures that allow this type of microemulsions to be achieved. with characteristic droplet sizes around ten microns. However, there is only one technique that can reduce the size below this level efficiently: that of simple and compound electrosprays (loscertales, Barrero and others, Science, (2002) 295, 5560). Here we present a technique that dispenses with the use of electric fields or surfactants and has such a simple geometry that it lacks the problems of centering the three-dimensional flow focusing devices, Gañán-Calvo and Gordillo, Phys. Rev. Lett. (2001), 87, 274501, or wetting with adjacent surfaces such as techniques that make use of flow-focusing devices created with soft-lithography methods (Anna et al, Appl. Phys. Lett, (2003), 82, 364-366). These methods, in addition to being more complex in terms of their geometry since the current to be dispersed has to be focused through an orifice or channel of smaller dimension than the injector needle, are unable to achieve droplet sizes below 5 microns systematically.
    In recent times, there is a growing interest on the part of the food, pharmaceutical or chemical industry to generate capsules that contain an active ingredient inside and that are externally coated with a flexible or rigid shell. There are innumerable patents that register a procedure for the production of capsules
    or of emulsions. In the case of capsules for food application are the examples of patents AU754712 and EP1263451. In applications to the chemical industry (mainly companies dedicated to the manufacture of detergents), EP1288287 and WO03002160. Applications to the pharmaceutical industry are the most common and have countless records, among which WO03004003, WO041740, US6514526, EP1151746. In most of these examples, the capsules are generated by chemical processes of deposition of a substance on the surface of a drop of a compound or active ingredient. The purpose of the outer shell, which is usually elastic or rigid, is to protect the active substance that is inside. There are procedures, initially patented at the University of Seville, which follow a different procedure to encapsulate liquids or generate emulsions.
    image3
    Both are based on coaxially flowing two immiscible fluid currents. It is well known that cylindrical jets break into droplets due to the growth of a hair instability, also known as Rayleigh instability. When this break occurs simultaneously in the inner and outer jets, drops are generated that have smaller droplets inside. If the outer shell is made solid by some method (for example, by making the outer fluid a photopolymer that increases its viscosity or stiffens with ultraviolet light), solid capsules can be generated. Emulsions can be generated in these devices by simply injecting a liquid using any of the procedures outlined above in a bath of an immiscible liquid with the injected fluid. The first procedure belongs to the family of devices known as flow focusing, and is protected by patents US 6174469, US 6187214 and US 6450189. In this case, as with the atomizers of the flow focusing type, the two concentric streams of fluid they are accelerated due to the favorable pressure gradient that exists between a pressurized chamber with gas and the outside. The diameter of the inner and outer jets decreases and, finally, by a fundamentally capillary mechanism, the compound drops are generated. These compound drops may have diameters of the order of 1 00 microns. On the other hand, with the technology known as Y-Flow, the inner and outer concentric jets are accelerated using an electric field. The capsules generated can have nanometric sizes (the capsules produced according to this procedure are the smallest ever generated), and are protected according to patents P200100231, PCT ES02 / 00047 and PCT US 02/02787. This procedure has, however, the disadvantage compared to flow focusing devices that electric fields are necessary and that the flow rates of the order are 1000 to 100 times smaller than those that can be used in flow focusing technology. Description of the figures
    To complement the description of the invention, and in order to help a better understanding of its characteristics, two planes are included in the present specification, as an integral part thereof, which are illustrative and not limiting, collect two models of prototypes of generating simple and compound emulsions (Fig. 1 and Fig. 2 respectively), as well as two image relationships that show the actual production of emulsions, both simple and compound (Fig. 3 and Fig. 4) with prototypes of the two lessons.
    Figure 1: The figure consists of the scheme of a prototype device for the generation of simple emulsions.
    The device is constituted by the injection tube (1) of the liquid to be emulsified, of internal diameter d¡, coaxially aligned and separated a distance h from the extraction tube (3), of length l and square section of inner side lo and outlet to exterior, contained inside a discharge chamber (4) with a hole (5) for the entry of the emulsifying liquid.
    Furthermore, to illustrate the generation of simple emulsions in the device by the method object of the invention, the velocity profile is shown in the figure.
    (6) of the flow of the liquid to be emulsified inside the injection tube, and the current lines (10) and the velocity profile (8) of the flow of the emulsifying liquid around the inlet section of the extraction tube and downstream inside, respectively.
    image4
    Figure 2: The figure is the schematic of a prototype device for generating composite emulsions.
    The different parts that comprise it are a composite injection tube formed by an inner capillary tube (1) of diameter d, for the injection of the inner liquid, coaxially centered inside a second outer capillary tube (2) of diameter d by where the intermediate liquid is injected, coaxially aligned and separated a distance h from the extraction tube (3), of length l and square section of the inner side and outflow, contained inside a discharge chamber (4) with a hole (5) for the entry of the emulsifying liquid.
    In addition, to illustrate the generation of compound emulsions in the device by means of the method object of the invention, the velocity profile of the flow of the inner liquid (6) inside the inner injection tube, the velocity profile of the interior is represented in the figure. intermediate fluid flow (7) inside the outer injection tube, and the flow lines (10) and the velocity profile (8) of the emulsifying liquid flow around the inlet section of the extraction tube and downstream inside, respectively.
    Figure 3: The image relationship of the figure shows the actual production of simple emulsions by the method object of the invention in a prototype of the device object of the invention with different geometric configurations of its components.
    The outer liquid is 100 cSt viscosity silicone oil and the distilled water inside (1 cSt viscosity). The flow of the external liquid is 900 ml / h and the flow of the internal liquid 0.5 ml / h, in all four cases.
    The geometric configuration of the devices in each of the images in the series is as follows: 3.1. - lo = 1 mm, di = 450 µm and h = 0.5 lo; 3.2. - di = 450 µm and h = 1.0 lo;
    3.3. - di = lo and h = 1.0 lo; 3.4 - di = lo and h = 1.5 lo. The internal dimensions of the four prototype drive chamber are 3 cm x 3 cm x 3 cm.
    Figure 4: The image relationship of the figure shows the production of compound emulsions by the method object of the invention in a prototype device object of the invention with the following geometric configuration of the elements that form it: di = 700 µm, do = 1.0 mm, lo = 10 mm and h = 1.70 mm. The interior dimensions of its discharge chamber are 3 cm x 3 cm x 3 cm.
    The outer liquid is silicone oil of 1000 cSt viscosity. The intermediate liquid is a mixture of glycerol and distilled water with a viscosity at 25 C of 400 cSt and the inner liquid is silicone oil of 10 cSt viscosity.
    The flow of the external liquid is 200 ml / h and the flow of the intermediate liquid is 200 ml / h. The flow of the inner liquid q; in each of the images of the series is the following:
    4.1. - qi = 0.10 ml / h; 4.2.- qi = 0.30 ml / h; 4.3. - qi = 0.50 ml / h; 4.4. - qi = 0.70 ml / h.
    image5 Description of the invention
    The object of the present invention is a method of generating simple and compound emulsions, from the formation of a capillary microchorr, simple or compound, as the case may be, when a liquid or two immiscible or barely miscible liquids flowing coaxially flows , by means of a viscous, immiscible or poorly miscible outer liquid with the simple or compound liquid to be emulsified, and flowing at the proper speed, as well as the device where and with which to carry out said procedure.
    According to a parametric determination, whose specification constitutes the essence of the process of the invention. in the case of generating simple emulsions, the suctioned liquid forms a stationary capillary jet of controllable diameter and micrometric size by the action of the outer liquid coflume and the favorable pressure gradient it produces. This simple jet breaks due to capillary instability producing micro and submicron droplets and low size dispersion.
    In the case of generation of compound emulsions, the suction causes a capillary jet composed, by the action of the coflujo of the external liquid and the favorable pressure gradient that it produces on the intermediate liquid and of this on the internal liquid in the same way. The interior of this compound jet breaks into droplets due to capillary instability, inducing the breakage of the intermediate liquid producing the coating of the drops of the inner liquid and with it the formation of compound drops, of micrometric size.
    The parametric determination in the generation of compound emulsions allows control of both the droplet size of the inner liquid and the thickness of its coating with the intermediate liquid.
    The process of the invention is applicable in all those technological demands that require the generation of simple monodisperse emulsions of micrometric sizes of the phase to be dispersed, as well as in those technological demands that require the generation of homogeneous compound emulsions, whose dispersed phase requires diameters drop and thickness of its coating of micrometric and controllable sizes.
    The object of the present invention is a method and a device for the generation of simple and compound emulsions of micrometric size.
    The device that produces the generation of emulsions is formed by the following elements: a discharge chamber of dimensions of the order of the centimeter, whose interior contains coaxially aligned tubes, an extraction tube, with an inner diameter or side lo and length l, and a simple injection capillary tube, of internal diameter di, or a composite injection capillary tube, formed by two concentric capillary tubes, the exterior of which has an internal size of 2 The outlet section of the simple or composite capillary tube is separated from the inlet section of the extraction tube a distance h. The geometric dimensions di, do, lo and h of the elements of the device constitute its geometric configuration.
    The geometric dimensions tested and that characterize the simple emulsion generation device are as follows: di is between 0.05 mm and 4 mm, it is between 0.05 mm and 4 mm, l is between 10 mm and 100 mm and h is between 0 mm and 4 mm. The geometric dimensions tested and that characterize the compound emulsion generation device are the following: d, it is between 0.1 mm and 1.4 mm, it is between 0.4 mm and 4 mm, it is between 0.05 mm and 4 mm, l is between 10 mm and 100 mm and h is between 0 mm and 4 mm.
    image6
    The circulation of a viscous outer liquid from the discharge chamber to the outside through the extraction tube produces in the surroundings of its inlet section the suction of the simple liquid li, injected into the chamber through the capillary tube through which it flows, forming a stationary capillary jet, which narrows downstream reaching a constant diameter of micrometric size. This jet is formed thanks to the action of the external fluid coflume and the favorable pressure gradient exerted by the external fluid on the single capillary jet. This simple jet breaks by capillary instability in drops of the same order as that of the jet that originates them, producing a simple monodispersed emulsion of micrometric size.
    If a composite injection capillary tube is used, the suction produces a capillary stream composed of the intermediate liquid, which forms the outermost crust of the jet, and the inner liquid, which is located in the center of the composite jet. The composite jet is formed thanks to the action of the coflujo of the external fluid and the favorable pressure gradient exerted by the external fluid on the intermediate fluid. The action of the outer coflujo and the favorable gradient of external pressures, together with the gradients of capillary pressures exerted by the intermediate fluid, also produce the formation of a capillary stream of the inner liquid, which by capillary instability breaks into drops that induce the rupture of the intermediate liquid causing its coating and with it the formation of compound droplets, producing a monodispersed composite emulsion of internal and external diameters and controllable coating thickness and micrometric sizes.
    The viscosities of the inner, intermediate and outer liquids, and the surface tensions between the inner and outer liquids, in the generation of simple emulsions and between the outer and intermediate and intermediate and inner liquids, in the generation of compound emulsions, are physical properties essential in the production of emulsions described in this invention and constitute what we will call its dimensional configuration.
    The flow rates of the internal, intermediate and external liquids, Qi, Qm and Qe respectively or, alternatively, the flow rates of the internal and intermediate liquids Qi and Qm respectively and the manometric pressure of the external fluid ∆pe, related to the external flow Qe of the form ∆pe = KQe, with K a constant that depends only on the geometry of the device, are the variables or parameters of operational control in the generation of emulsions produced by this technology and constitute what we will call its operational configuration.
    The method object of the present invention consists in the appropriate selection of the indicated geometric, dimensional and operational parameters or variables, that is to say in the specification of the geometric, dimensional and operational configurations.
    image7
    The specification of the geometric dimensional and operational configurations define a parametric determination or a mode of production.
    The following formulations express the physics of the phenomenon on which the described technology is based:
    (i) .- The Reynolds numbers characteristic of the outer and inner stream are less than 1 and less than 10, respectively: ρoUoD / µo <1 and ρiQi / (Dµo) <10, where Uo is the velocity of the outer fluid in the center of the extraction tube
    (ii) .- the capillary number is greater than 0.75; µoUo / σ> 0.75
    (iii) .- the flow rate of the inner liquid and the velocity of the outer liquid are such that [4Qi / (π Uo)] ½ <1 mm.
    If the parametric determination or the mode of production chosen satisfies each of the previous numerical relationships, then the generation of simple emulsions by this device and procedure is feasible. In this case, the scale law that predicts the size of the diameter of the drops that form the emulsion is as follows: 0.25 [4Qi / (πUo)] ½ <d <4 [4Qi / (πUo)] ½. In the event that the emulsion is composed, Qi in the previous equation must be replaced by Qi + Qm.
    The invention described herein has application in those industrial sectors in which the production of simple and homogeneous, homogeneous and compound emulsions with controllable diameters and coatings of micrometer size is an essential part of the process. Embodiment of the invention
    Example of embodiment of the invention for the generation of simple emulsions.
    Image 3.2 of Figure 3 of the present specification shows the actual production of simple emulsions by this invention. In addition, the scheme of the device used is presented in Figure 1.
    The prototype is constituted by a discharge chamber (4) of internal dimensions 3 cm x 3 cm x 3cm, which contains inside an extraction tube (3) of square and glass section, with an inner side lo = 1 mm and length l = 4 cm, and a single injection capillary tube (1), made of stainless steel and with an internal diameter of di = 450 µm. The separation between both tubes is h = 1 mm.
    The drive chamber contains two pairs of windows, to allow real-time monitoring of the production of simple emulsions.
    The outer and inner liquids used in this embodiment of the invention for the generation of simple emulsions are 100 cSt silicone oil and distilled water (1 cSt viscosity) respectively, with surface tension between them of 40 mN / m.
    The flow rates of the outer and inner liquids, Qe and Qi, have been varied between 450 ml / h and 1400 ml / h and 0.1 ml / h, respectively, producing drop emulsions of sizes between 10 µm and 100 µm, with a production frequency between 1000 Hz and 10000 Hz.
    image8
    Image 3.2 of Figure 3 illustrates the real simple emulsion produced according to the previous specifications with the injection of flow rates Qe = 1150 ml / h and Qi = 0.5 ml / h. The remaining images of the series, that is images 3.1, 3.3 and 3.4 of Figure 3 show the actual simple emulsions according to different geometric configurations, and without changing the rest of the specifications of the production mode described above.
    To evaluate the versatility of both the procedure and the device for generating simple emulsions, as well as the amplitude of the parametric determination, emulsions have been produced by modifying:
    (i)  the different variables that characterize the geometric configuration of its elements (do, h, lo and l),
    (ii)  the viscosity of the outer and inner liquid in the ranges between 100 cSt and 1000 cSt and between 1 cSt and 1 cSt respectively, and the surface tension between them between 1 mN / m and 40 mN / m, replacing some liquids with others of different properties,
    (iii) and the specific and specific values of the operative control parameters of the production of simple emulsions, that is to say, the flows of external and internal liquid, in the ranges between 100 ml / h and 4000 ml / h and 0.01 ml / h and 100 ml / h respectively.
    In each case, the existence of a parametric window is checked in which the production of emulsions is effective, continuous, uniform and stable.
    Example of embodiment of the invention for the generation of compound emulsions.
    Image 4.2 of Figure 4 of the present specification shows the actual production of compound emulsions by this invention. In addition, the scheme of the device used is presented in Figure 2.
    The prototype is made up of a 3 cm x 3 cm x 3 cm internal drive chamber, which contains an extraction tube (4) with a square and glass section inside, with an inner side lo = 1 mm and length l = 4 cm, and a composite injection tube, formed by a capillary tube (1) through which the inner liquid circulates, of diameter di = 450 µm, contained and coaxially centered inside a second capillary tube (3) in diameter inside do = 1.20 mm, through which the intermediate liquid flows. The separation between both tubes is h = 1 mm.
    The drive chamber contains two pairs of windows, to allow real-time monitoring of the production of simple emulsions.
    The outer, intermediate and inner liquids used in this embodiment of the invention for the generation of compound emulsions are 1000 cSt silicone oil, a mixture of glycerin and distilled water with a viscosity at 25 C of 400 cSt and silicone oil of 10 cSt viscosity, respectively, with surface tension between both pairs of liquids (exterior and intermediate and intermediate and internal) of 50 mN / m.
    image9
    The flow rates of the outer, intermediate and inner liquids, Qe, Qm and Qi, have been varied between 100 ml / h and 200 ml / h, 0.1 ml / h and 10.0 ml / h and 0.1 ml / h and 10 ml / h, respectively, producing drop emulsions composed of inner diameter sizes between 10 µm and 100 µm, and coatings between 10 µm and 40 µm, with a production frequency between 100 Hz and 2000 Hz.
    Image 4.2 in Figure 4 shows the production of a compound emulsion according to the previous specifications, in the case of Qe = 200 ml / h, Qm = 2ml / h and Qi = 0.5 ml / h. The rest of the series images, that is images 4.1, 4.3 and 4.4 of Figure 4 show the real production of emulsions composed according to different flow rates of the inner liquid, between 0.1 ml / h and 0.7 ml / h, without changing the rest of specifications of the production mode described above.
    To evaluate the versatility of both the process and the compound emulsion generation device, as well as the amplitude of the parametric determination, emulsions have been produced by modifying:
    (i)  the different variables that characterize the geometric configuration of its elements (do, h, lo and l),
    (ii)  the viscosity of the outer liquid, in the range between 100 cSt and 1000 cSt, the viscosity of the intermediate liquid between 50 cSt and 1000 cSt, the viscosity of the inner liquid between 1 cSt and 20 cSt, the surface tension between both liquids between 20 mN / m and 50 mN / m, by replacing some liquids with others of different properties,
    (iii) and the specific and specific values of the operative control parameters of the production of the compound emulsions, that is to say, the flows of external, intermediate and internal liquid, in the ranges between 100 ml / h and 4000 ml / h, between 0.01 ml / h and 10 ml / h and between 0.01 ml / h and 100 ml / h respectively
    In each case, the existence of a parametric window is checked in which the production of emulsions is effective, continuous, uniform and stable.
    The materials from which the different elements that constitute the simple and compound emulsion generator can be manufactured are multiple (metal, plastic, ceramic, glass), fundamentally depending on the choice of material for the specific application in which the material is to be used. device.
    Any methods of continuous supply of the external, intermediate and internal liquids (pressure tanks, syringe pumps, etc.) can be used.
    The foregoing examples of embodiment of the invention describe the method and the individual device or cell for generating simple or compound emulsions with the limitation of the production involved. If an increase in production is required, the device can be multiplexed. In this case, the flow of internal liquid or intermediate and internal liquids, as the case may be, should be as homogeneous as possible between the different cells, which may require impulsion through multiple capillary needles, porous media, or any other medium capable of distributing a homogeneous flow rate between different feeding points.
    权利要求:
    Claims (24)
    [1]
    image 1
    1. Device for generating simple emulsions, consisting of an injection tube (1), of internal diameter di, coaxially aligned and separated a distance h from an extraction tube (3), of length l and circular or square section of diameter or inner side lo and outside exit, contained inside a drive chamber (4), characterized in that
    1st.- di is between 0.05 mm and 4 mm,
    1b.- lo and l are between 0.05 mm and 4 mm, and 10 mm and 100 respectively and
    1c.- h is between 0 mm and 4 mm.
    [2]
    2.  Simple emulsion generation device according to claim 1, characterized in that 2a.- di is between 0.40 mm and 1.40 mm,
    2b.- lo and l are between 0.70 mm and 1.20 mm, and 20 mm and 50 respectively and 2c.- h is between 0.50 mm and 1 50 mm.
    [3]
    3.  Composite emulsion generating device, consisting of an injection tube composed of an inner capillary tube (1) of internal diameter di, coaxially centered inside a second outer capillary tube (2) of internal diameter do, coaxially aligned and separated a distance h from a tube of an extraction tube (3), of length l and circular or square section of diameter or inner side lo and exit to the outside, contained inside a discharge chamber (4), characterized in that
    3a.- di is between 0.10 mm and 1.40 mm,
    3b.- do is between 0.40 and 4 mm,
    3c.- lo and l are between 0.05 mm and 4 mm, and 10 mm and 100 respectively and
    3d.- h is between 0 mm and 4 mm.
    [4]
    Four.  Composite emulsion generation device according to claim 3, characterized in that 4a.- di is between 0.30 mm and 0.70 mm, 4b.- do is between 0.70 mm and 1.40 mm,
    4c.- lo and l are between 0.70 mm and 1.20 mm, and 20 mm and 50 respectively and 4d.- h is between 0.50 mm and 1 50 mm.
    [5]
    5.  Device for generating simple emulsions according to claims 1 and 2, characterized in that the different parts that comprise it are made of various materials such as metal, plastic, ceramic, glass or others.
    [6]
    6.  Composite emulsion generation device according to claims 3 and 4, characterized in that the different parts that compose it are made of various materials such as metal, plastic, ceramic, glass or others.
    [7]
    7.  Simple emulsion generation device according to claims 1, 2 and 5, characterized in that the drive chamber has windows that allow real-time monitoring of emulsion production, as well as the study of the physical phenomenon that supports it.
    [8]
    8.  Composite emulsion generation device according to claims 3, 4 and 6, characterized in that the drive chamber has windows that allow real-time monitoring of emulsion production, as well as the study of the physical phenomenon that supports it.
    [9]
    9.  Multiplexed device for generating simple emulsions, characterized in that each of the individual cells that comprise it has the technical characteristics described in claims 1, 2, 5 and 7.
    [10]
    10.  Multiplexed device for generating composite emulsions, characterized in that each of the individual cells that comprise it has the technical characteristics described in claims 3, 4, 6 and 8.
    [11]
    eleven.  Simple emulsions of any two immiscible or poorly miscible fluids with each other, characterized in that the diameters d of the drops produced by an emulsion generating device with the technical characteristics described in claims 1, 2, 5, 7 and 9 satisfy the 025 ratio [4Qi / (πUo)] ½ <d <4 [4Qi / (πUo)] ½, where Qi is the flow of the inner liquid and Uo the velocity of the emulsifying liquid in the center of the capillary tube.
    [12]
    12.  Emulsions composed of any two immiscible or barely miscible fluids with each other emulsified by any immiscible or barely miscible fluid with the exterior of the above, characterized in that the diameters d of the drops produced by means of an emulsion generating device with the technical characteristics described in the claims 3, 4, 6, 8 and 10 satisfy the ratio 0.25 [4 (Qi + Qm) / (πUo)] ½ <d <4 [4 (Qi + Qm) / (πUo)] ½ where Qi is the liquid flow inside, Qm the flow of the intermediate liquid and Uo the speed of the emulsifying liquid in the center of the capillary tube.
    [13]
    13.  Method of generating simple emulsions of micrometer size, characterized in that a flow of liquid Qi is injected through a needle of internal diameter d1 into a chamber to which a flow Qe of an emulsifying liquid of viscosity greater than that of the liquid to be emulsified, this pair of liquids being immiscible or barely miscible with each other, and said chamber having a capillary extraction needle of length l and of a characteristic transverse dimension located at a distance h from the outlet of the injection needle, with di, lo, lyh according to claims 1, 2, 5 and 7, and the purpose of the extraction needle being to generate a favorable pressure gradient along its entire length
    on the liquid to be emulsified and on the emulsifier, a capillary jet of stable micrometric size being formed inside the extraction tube that disintegrates into drops of uniform sizes thanks to the growth of a capillary instability.
    [14]
    14.  Method of generating simple emulsions of micrometric size according to claim 13, characterized in that
    image2
    image3
    14a.- the viscosity of the liquid to be emulsified is between 1 cSt and 1000 cSt and the viscosity of the emulsifying liquid is between 1 cSt and 10000 cSt;
    14b.- the flow rate of liquid to be emulsified Qi is comprised between 0.01 ml / h and 100 ml / h and the flow rate of the emulsifying liquid Qe is comprised between 1 and 4000 ml / h;
    [15]
    15. Method of generating simple emulsions of micrometric size according to claim 13, characterized in that
    15a.- the viscosity of the liquid to be emulsified is between 1 cSt and 50 cSt and the viscosity of the emulsifying liquid is between 50 cSt and 1000 cSt;
    15b.- the flow of liquid to be emulsified is between 0.1 ml / h and 10 ml / h and the flow of the emulsifying liquid is between 50 ml / h and 1000 ml / h.
    [16]
    16.  Method of generating simple emulsions of micrometric size according to claims 13 and 14 which is implemented using a simple emulsion generating device with the technical characteristics described in claim 9, in this case the flow rates described in claim 14b being those corresponding to an individual cell of the multiplexed device
    [17]
    17.  Procedure for generating compound emulsions of micrometric size. characterized in that a flow of internal liquid Qi and a flow rate Qm of an intermediate liquid that is immiscible or poorly miscible with the first are injected through a capillary needle composed of two coaxial tubes of respective internal diameters di and do within a chamber to which a flow rate Qe of an emulsifying liquid of viscosity greater than that of the emulsifying and immiscible liquids is supplied
    or poorly miscible with the intermediate liquid, said chamber having an extraction capillary tube of length l and of a characteristic transverse dimension located at a distance h from the outlet of the composite capillary tube, with di, do, lo, lyh according to claims 3 , 4, 6 and 8, and the purpose of the extraction needle is to generate along its entire length l> lo a favorable pressure gradient on the liquids to be emulsified and on the emulsifier, resulting in a capillary jet composed of the inner and intermediate liquids of micrometric outer size that disintegrates into drops composed of the inner and intermediate liquids of uniform sizes thanks to the growth of a capillary instability.
    [18]
    18. Composite emulsion generation method according to claim 17, characterized in that
    18a.- the viscosity of the inner liquid (li) of the composite jet to be emulsified is between 1 cSt and 1000 cSt, the viscosity of the outer liquid of the composite jet (lm) to be emulsified is between 1 cSt and 1000 cSt and the viscosity of the emulsifying liquid (le) is between 1 cSt and 1000 cSt;
    image4
    18b.- the flow rate Qi of the inner liquid of the composite jet to be emulsified is between 0.01 ml / h and 100 ml / h, the flow rate Qm of the outer liquid of the composite jet to be emulsified is between 0.001 ml / h and 1000 ml / h Qe of the emulsifying liquid is between 1 ml / h and 4000 ml / h;
    [19]
    19. Composite emulsion generation method according to claim 17, characterized in that
    19a.- the viscosity of the liquid li is between 1cSt and 10 cSt, the viscosity of the liquid lm is between 10 cSt and 100 cSt and the viscosity of the liquid is between 100 cSt and 1000 cSt;
    19b.- the flow rate of the liquid li is between 0.1 ml / h and 10 ml / h, the flow rate of the liquid lm is between 0.01 ml / h and 100 ml / h and the flow rate of the liquid is between 50 ml / h and 1000 ml / h.
    [20]
    twenty.  Method of generating composite emulsions of micrometer size according to claim 17 and 18 implemented using a compound emulsion generating device with the technical characteristics described in claim 10, in this case the flow rates described in claim 18b being those corresponding to a cell individual multiplexed device.
    [21]
    twenty-one.  Method of generating composite emulsions according to claim 17, characterized in that
    21a.- the viscosity of the liquid li is between 1 cSt and 10 cSt, the viscosity of the liquid lm is between 100 cSt and 400 cSt and the viscosity of the liquid is between 400 cSt and 1000 cSt;
    21b.- the flow rate of the liquid li is between 0.1 ml / h and 10 ml / h, the flow rate of the liquid lm is between 0.01 ml / h and 100 ml / h and the flow rate of the liquid is between 50 ml / h and 1000 ml / h.
    [22]
    22. Composite emulsion generation method according to claim 17, characterized in that
    22a.- the viscosity of the liquid li is between 1 cSt and 10 cSt, the viscosity of the liquid lm is between 400 cSt and 700 cSt and the viscosity of the liquid is between 700cSt and 1000 cSt;
    22b.- the flow rate of the liquid li is between 0.1 ml / h and 10 ml / h, the flow rate of the liquid lm is between 0.01 ml / h and 100 ml / h and the flow rate of the liquid is between 50 ml / h and 1000 ml / h.
    [23]
    2. 3.  Simple emulsions of any two immiscible or poorly miscible fluids with each other, characterized in that the diameters d of the drops produced by the emulsion generation method described in claims 13, 14, 15 and
    16 satisfy the ratio 025 [4Qi / (πUo)] ½ <d <4 [4Qi / (πUo)] ½, with Qi being the flow of the inner liquid and Uo the speed of the emulsifying liquid in the center of the capillary tube.
    [24]
    24.  Emulsions composed of any two immiscible or sparingly fluids
    image5
    5 miscible with each other emulsified by any immiscible fluid or poorly miscible with the outside of the foregoing, characterized in that the diameters d of the drops produced by the emulsion generation process described in claims 17, 18, 19, 20, 21 and 22 satisfy the ratio 0.25 [4 (Qi + Qm) / (πUo)] ½ <d <4 [4 (Qi + Qm) / (πUo)] ½ where Qi is the flow of the inner liquid, Qm the flow of the liquid
    10 intermediate and Uo the speed of the emulsifying liquid in the center of the capillary tube.
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    同族专利:
    公开号 | 公开日
    WO2016030551A1|2016-03-03|
    ES2564893B2|2016-07-08|
    EP3187252A1|2017-07-05|
    EP3187252A4|2018-02-14|
    EP3187252B1|2020-12-30|
    ES2872473T3|2021-11-02|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    ES2283158B1|2003-11-10|2008-09-16|Universidad De Sevilla|PROCEDURE AND DEVICE FOR THE GENERATION OF FOAMS AND EMULSIONS THROUGH PAIRS OF FACED TUBES.|
    US9039273B2|2005-03-04|2015-05-26|President And Fellows Of Harvard College|Method and apparatus for forming multiple emulsions|
    WO2013006661A2|2011-07-06|2013-01-10|President And Fellows Of Harvard College|Multiple emulsions and techniques for the formation of multiple emulsions|CN110869114A|2017-07-04|2020-03-06|布鲁塞尔自由大学|Droplet and/or bubble generator|
    CN108159976A|2018-01-03|2018-06-15|西南交通大学|A kind of Water-In-Oil Bao Shui（W/W/O）Monodisperse double emulsion preparation method and its micro fluidic device|
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    PCT/ES2015/000113| WO2016030551A1|2014-08-25|2015-08-25|Method and device for producing simple and compound micrometre-sized emulsions|
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