A 3D microemulsion preparation device and preparation method

Abstract

The present application discloses a 3D microemulsion preparation device and a preparation method. The 3D microemulsion preparation device includes a preparation cavity provided on a preparation body, transparent windows are provided on the front and rear sides of the preparation cavity, a top exhaust pipe, a feeding side conveying pipe, a collecting side conveying pipe and a generating side conveying pipe are provided on the preparation body, the four pipes are connected to the preparation cavity, and the ends of the four pipes away from the preparation cavity are detachably connected to plugs; when in use, the preparation body is placed vertically, the plugs above, below and on the collecting side of the preparation cavity are removed, the continuous phase is introduced into the preparation cavity through the feeding side conveying pipe, the top exhaust pipe is blocked after it is full, the plug installed on the generating side conveying pipe is removed, the dispersed phase is introduced through the generating side conveying pipe, and the flow rates of the dispersed phase and the continuous phase are adjusted to prepare microemulsions of different sizes and frequencies. The overall structure is simple, easy to observe, simple to operate and use, and can reduce preparation costs and simplify the preparation process.

Description

Technical Field

[0001] The present application relates to the technical field of microemulsion preparation, and in particular to a preparation device and method for preparing microemulsions and microparticles that can be used in the fields of materials science, biomedicine, synthesis and screening of new drugs, food and commodity inspection, military science, aerospace science, etc. Background Art

[0002] Microemulsion droplets are a uniquely structured liquid system in which oil, water, and surfactants (sometimes with co-surfactants) form stable droplets under specific conditions. These droplets are nanometer- or micrometer-sized and can be uniformly dispersed in a mixed solvent. Microemulsions offer many advantages, including high surface area, high-throughput processing, independent reaction chambers, rapid mixing and heat transfer, and the ability to function as microreactors.

[0003] The preparation methods of microemulsions mainly include early high-speed stirring, layer-by-layer assembly technology, membrane emulsification method and other preparation methods, as well as the currently more commonly used preparation methods based on microfluidic systems. Early high-speed stirring, layer-by-layer assembly technology, membrane emulsification method and other preparation methods have fewer steps, simple operation and strong versatility. The preparation method based on the microfluidic system provides a more precise control means. This method can obtain spherical particles with uniform particle size distribution through the microfluidic system, and the prepared microemulsions have good stability when stored at room temperature, and the particle size changes little in a short period of time. For example, Chinese invention patent CN113136421A discloses a microemulsion of a W / O / W type PCR amplification product based on a microfluidic system and its preparation method. This document is based on the microfluidic system to prepare microemulsions.

[0004] Although microemulsions can be produced by the above-mentioned preparation methods, they still have the following defects in actual production: although the early preparation methods are simple to operate, the uniformity of the microemulsions produced is poor and the experimental repeatability is low, that is, the quality of the microemulsion preparation is not high. The method of preparing microemulsions based on microfluidic systems is mainly based on microfluidic chips, which have the following disadvantages in application: 1) Traditional microfluidic chips are usually 2D structures, which are made by two plates, one of which has a groove engraved on it and then bonded (glued) to the other plate. Traditional 2D microfluidic chips are affected by the material properties of the inner wall of the chip microchannel, and many solutions cannot interact to form microemulsions; 2) Existing microfluidic chips have problems such as easy clogging, difficult cleaning, slow generation rate, and difficulty in generating multiple emulsions; 3) Microfluidic chips require complex surface modification (hydrophilic and hydrophobic modification) according to the different types of microemulsion structures to be generated; In short, the cost of preparing microemulsions is high and the preparation process is complicated. Therefore, the current preparation cost of microemulsions is high, the preparation process is complex, and many solutions cannot be generated into microemulsions using the principle of microfluidic chips. Therefore, it is necessary to propose a new technical solution to solve the problems existing in the existing technology. Summary of the Invention

[0005] The present application provides a 3D microemulsion preparation device and preparation method to solve the problems of high cost and complex preparation process of microemulsion preparation in the prior art.

[0006] In order to achieve the above objectives, this application provides the following technical solutions:

[0007] On the one hand, the present application provides a 3D microemulsion preparation device, including a preparation body, a through hole is opened on the preparation body, and transparent windows are installed at both ends of the through hole respectively, the channel of the through hole and the two transparent windows together form a preparation cavity, and a generation nozzle and a collecting device arranged opposite to the generation nozzle are provided in the preparation cavity, and the collecting device is a collection tube or a collection nozzle; a top exhaust pipe, a feeding side delivery pipe for adapting and connecting to a capillary through which a continuous phase passes, a collecting side delivery pipe for adapting and connecting to a collecting capillary, and a generation side delivery pipe for adapting and connecting to a capillary through which a dispersed phase passes are provided on the preparation body; the top exhaust pipe, the feeding side delivery pipe, the collecting side delivery pipe and the generation side delivery pipe are respectively connected to the preparation cavity, the generation side delivery pipe is connected to the generation nozzle, and the collecting device is connected to the collection side delivery pipe; the top exhaust pipe, the feeding side delivery pipe, the collecting side delivery pipe and the generation side delivery pipe are respectively detachably connected to the plug at one end away from the preparation cavity.

[0008] Furthermore, in the above technical solution, the preparation body is a block structure, the through hole is a through hole opened at the center position of the preparation body, and along the length direction of the through hole, the two opposite side walls of the preparation body are respectively provided with installation grooves for installing the transparent window, the cross-sectional area of ​​the bottom of the installation groove is larger than the cross-sectional area of ​​the through hole, and the bottom of the installation groove is connected to the through hole.

[0009] Furthermore, the transparent window includes a glass plate and a cover plate covered on the glass plate. The glass plate is embedded in the installation groove. An observation hole is opened at the center of the cover plate. The cover plate is located on the side of the glass plate away from the through hole. The observation hole corresponds to the through hole. A plurality of fixing holes for installing screws are set on the edge of the cover plate. The cover plate is detachably connected to the preparation body by screws.

[0010] Furthermore, the generating side conveying pipeline and the collecting side conveying pipeline are arranged opposite to each other in the horizontal direction, and the generating nozzle and the collecting pipe or the collecting nozzle are arranged opposite to each other in the horizontal direction; the top exhaust pipeline and the feeding side conveying pipeline are arranged opposite to each other in the vertical direction, and the top exhaust pipeline is located above the feeding side conveying pipeline.

[0011] Furthermore, a first connecting groove is formed at one end of the top exhaust pipe away from the preparation chamber, which is adapted to be plugged into the first plug; a second connecting groove is formed at one end of the feed side delivery pipe away from the preparation chamber, which is adapted to be plugged into the second plug, and the second connecting groove is detachably connected to the capillary tube through which the continuous phase passes through a connecting joint and a gasket.

[0012] Furthermore, a generation side assembly groove is provided on the side wall of the preparation body on which the generation side delivery pipeline is provided, a generation side plug is adapted to be installed in the generation side assembly groove, a generation side flow channel is provided on the generation side plug, and the generation side flow channel is connected to the generation side delivery pipeline; a generation side baffle is provided on the preparation body, the generation side baffle is detachably connected to the preparation body by screws, the generation side baffle can encapsulate the generation side plug in the generation side assembly groove, a baffle channel corresponding to the generation side flow channel is provided on the generation side baffle, and the baffle channel is detachably connected to the third plug; a sealing groove is provided on the side wall where the generation side plug is connected to the generation side baffle, a sealing ring is provided in the sealing groove, and the end of the baffle channel connected to the generation side flow channel abuts against the sealing ring.

[0013] Furthermore, a collecting side assembly groove is provided on the side wall of the preparation body on which the collecting side conveying pipe is provided, a collecting side plug is adapted to be installed in the collecting side assembly groove, a collecting side flow channel is provided on the collecting side plug, and the collecting side flow channel is connected to the collecting side conveying pipe; a collecting side baffle is provided on the preparation body, the collecting side baffle is detachably connected to the preparation body by screws, the collecting side baffle can encapsulate the collecting side plug in the collecting side assembly groove, a baffle channel corresponding to the collecting side flow channel is provided on the collecting side baffle, and the baffle channel is detachably connected to the fourth plug; a sealing groove is provided on the side wall where the collecting side plug is connected to the collecting side baffle, a sealing ring is provided in the sealing groove, and the end of the baffle channel connected to the collecting side flow channel abuts against the sealing ring.

[0014] Furthermore, the material of the generating nozzle and the material of the collecting device are adapted to the chemical solution used to prepare the microemulsion droplets to ensure compatibility and performance.

[0015] Furthermore, the material of the generating nozzle is glass, polymer material, ceramic or metal, and the inner diameter of the generating nozzle ranges from 10 μm to 1 mm.

[0016] Furthermore, the material of the collecting tube or the collecting nozzle is glass, polymer material, ceramic or metal, and the inner diameter of the collecting tube or the collecting nozzle ranges from 10 μm to 1 mm.

[0017] Furthermore, the installation distance between the generating nozzle and the collecting device ranges from 10 μm to 500 μm.

[0018] On the other hand, the present application provides a method for preparing microemulsion droplets, using the above-mentioned 3D microemulsion preparation device, the microemulsion preparation method comprises the following steps:

[0019] S1: Remove all the plugs installed on the top exhaust pipe, the feeding side conveying pipe and the collection side conveying pipe;

[0020] S2: fixedly connecting the capillary tube with the continuous phase to the feeding side delivery pipe, fixedly connecting one end of the collecting capillary tube to the collecting side delivery pipe, and connecting the other end of the collecting capillary tube to the collection container;

[0021] S3: Place the preparation body vertically so that the top exhaust pipe is above the preparation chamber, and introduce the continuous phase into the preparation chamber at the target flow rate. Observe the filling process of the continuous phase in the preparation chamber through the transparent window. When the preparation chamber is full of the continuous phase, plug the top exhaust pipe with a plug and reduce the flow rate of the continuous phase.

[0022] S4: Remove the plug installed on the generation side delivery pipeline, fix the capillary tube with the dispersed phase to the generation side delivery pipeline, introduce the dispersed phase into the preparation cavity at a target flow rate, generate microemulsion droplets of target size and target frequency distribution in the preparation cavity, and the generated microemulsion droplets are sent to the collection container through the collection tube in the preparation cavity.

[0023] In step S3 of the microemulsion preparation method, if bubbles are generated during the filling process of the continuous phase, the preparation body is gently shaken to allow the air in the preparation body to be discharged from the top exhaust pipe to eliminate the bubbles.

[0024] Furthermore, in the above-mentioned method for preparing microemulsions, microemulsions of different sizes and different frequency distributions are generated by adjusting the flow rate of the dispersed phase and / or the flow rate of the continuous phase introduced into the preparation cavity.

[0025] Compared with the prior art, this application has at least the following beneficial effects:

[0026] 1. The 3D microemulsion preparation device provided in the present application has a simple structure, low manufacturing, use and maintenance costs, a transparent window is provided for easy observation of the preparation process, and the operation and use are simple; using the device to prepare microemulsions can simplify the operating process, and when in use, microemulsions of different sizes and different frequency distributions can be generated by adjusting the flow rate of the dispersed phase and / or the flow rate of the continuous phase introduced into the preparation cavity. This flexible adjustment capability enables the device to meet different application requirements, thereby improving the applicability and flexibility of the microemulsion preparation device. Therefore, using the microemulsion preparation device provided in the present application can reduce preparation costs and simplify the preparation process.

[0027] 2. The 3D microemulsion preparation device provided in this application is provided with a preparation cavity on the preparation body, and transparent windows are provided on the front and back sides of the preparation cavity to facilitate observation and monitoring.

[0028] 3. The preparation body of the present application is provided with a top exhaust pipe, a feeding side conveying pipe, a collecting side conveying pipe, and a generating side conveying pipe. The four pipes are connected to the preparation cavity, and the ends of the four pipes away from the preparation cavity are detachably connected to the plugs, which are easy to install and use and the microemulsion preparation operation is simple.

[0029] 4. When preparing microemulsions using the 3D microemulsion preparation device, the preparation body is placed vertically, the plugs installed on the top exhaust pipe, the feeding side delivery pipe and the collecting side delivery pipe are removed, the capillary with the continuous phase is connected to the feeding side delivery pipe, the collecting capillary and the collection container are connected to the collecting side delivery pipe, and the continuous phase is introduced into the preparation cavity. During the filling process, the bubbles can be eliminated by shaking the preparation body. When the preparation cavity is full of the continuous phase, the top exhaust pipe is blocked with the plug, and the flow rate of the continuous phase is reduced. Then, the plug installed on the generation side delivery pipe is removed, and the capillary with the dispersed phase is fixedly connected to the generation side delivery pipe, and the dispersed phase is introduced into the preparation cavity at a target flow rate to generate microemulsions of target size and target frequency distribution in the preparation cavity. The generated microemulsions are sent to the collection container through the collection pipe in the preparation cavity. It can be seen that the device is easy to operate and the microemulsion preparation process is simple.

[0030] 5. In the 3D microemulsion preparation device provided in the present application, the generation nozzle and the collection tube or the collection nozzle are suspended in the preparation cavity and a spacing is left in the middle according to the design (the installation spacing range is 10μm to 500μm), so that the microemulsions are in a 3D free sphere state during generation and collection, which is conducive to the generation of microemulsions, solves the problem that some solutions cannot pass through the microfluidic chip to generate microemulsions, and ensures the stability of the microemulsions.

[0031] 6. In the 3D microemulsion preparation device provided in this application, all liquid contact materials are made of stainless steel, ceramics and other materials, which have good corrosion resistance, solving the problem that traditional microfluidic chips using PDMS, plastic, glass and other materials cannot adapt to highly corrosive materials.

[0032] 7. The 3D microemulsion preparation device provided in this application adopts a modular design and consists of a preparation cavity, a material input end, a material collection end, a microemulsion generation nozzle, a microemulsion collection tube or collection nozzle, a capillary joint, an observation window and other parts. All parts can be disassembled, cleaned and reused, which solves the problem of microfluidic chips being scrapped due to blockage and reduces preparation costs.

[0033] 8. The 3D microemulsion preparation device provided in this application adopts standard microfluidic connectors (1 / 4-28 or 10-1 / 32) and standard capillaries (1 / 16 inch or 1 / 32 inch), and adopts unidirectional linear connection, which is simple to connect, has good sealing, and ensures good repeatability of preparation; this solves the problem of difficult connection and leakage between the microfluidic chip and the capillary, and more importantly, solves the problem of microemulsion fusion or rupture caused by the vertical connection method commonly used in microfluidic chips. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work. It should be understood that the specific shapes and structures shown in the drawings should not generally be regarded as limiting conditions for implementing the present application; for example, based on the technical concepts and exemplary drawings disclosed in this application, those skilled in the art are able to easily make routine adjustments or further optimizations to the addition / reduction / attribution division, specific shapes, positional relationships, connection methods, and dimensional ratios of certain units (components).

[0035] Figure 1 This is a schematic diagram of the three-dimensional structure of the 3D microemulsion preparation device provided by the present application when placed vertically in an embodiment;

[0036] Figure 2 This is a schematic diagram of the structural disassembly of a 3D microemulsion preparation device provided by the present application in one embodiment;

[0037] Figure 3 This is a schematic diagram of the three-dimensional structure of the 3D microemulsion preparation device provided by the present application when placed horizontally in one embodiment;

[0038] Figure 4 for Figure 1 The schematic diagram of the front structure of the 3D microemulsion preparation device is shown;

[0039] Figure 5 for Figure 1 The left side structural schematic diagram of the 3D microemulsion preparation device is shown;

[0040] Figure 6 for Figure 1 The schematic diagram of the top view of the 3D microemulsion preparation device is shown.

[0041] Description of reference numerals:

[0042] 1. Prepare the body; 2. Through-hole; 3. Glass plate; 4. Cover plate; 5. Prepare the cavity; 6. Generate the nozzle; 7. Collecting tube; 8. First plug; 9. Second plug; 10. Third plug; 11. Fourth plug; 12. Generate the side assembly groove; 13. Generate the side plug; 14. Generate the side baffle; 15. Collecting side plug; 16. Collecting side baffle; 17. Seal ring;

[0043] A. Top exhaust pipe; B. Feeding side conveying pipe; C. Collection side conveying pipe; D. Generation side conveying pipe. DETAILED DESCRIPTION

[0044] The present application will be further described below in detail through specific embodiments in conjunction with the accompanying drawings.

[0045] In the description of this application: unless otherwise specified, the meaning of "plurality" is two or more. The terms "first", "second", "third", etc. in this application are intended to distinguish the objects referred to and do not have any special meaning in terms of technical connotation (for example, they should not be understood as emphasizing the importance or order, etc.). Expressions such as "including", "comprising", "having", etc. also mean "not limited to" (certain units, components, materials, steps, etc.).

[0046] Terms such as "upper," "lower," "left," "right," and "center" used in this application are generally intended to facilitate intuitive understanding when compared with the accompanying drawings and are not intended to be absolute limitations on positional relationships in actual products. Changes to these relative positional relationships are considered within the scope of this application without departing from the technical concepts disclosed herein.

[0047] Example 1

[0048] The present invention provides a 3D microemulsion preparation device. Figure 1 、 2 The device mainly comprises a preparation body 1, which serves as the structural mounting base of the device. Specifically, a through hole 2 is formed in the preparation body 1, with transparent windows installed at both ends of the through hole 2. The through hole 2 and the two transparent windows together form a preparation cavity 5, which is the microemulsion generation cavity of the device. The preparation cavity 5 is provided with a generation nozzle 6 and a collection device arranged opposite the generation nozzle 6, which is a collection tube or a collection nozzle. The preparation body 1 is also provided with four pipes, which are respectively connected to the preparation cavity 5. Feeding, exhaust, microemulsion generation and microemulsion collection are achieved through the four pipes. The four pipes are: top exhaust pipe A, feeding side delivery pipe B, collection side delivery pipe C and generation side delivery pipe D, wherein: the top exhaust pipe is provided at the top of the preparation body 1 to achieve the discharge of gas in the cavity during feeding; the feeding side delivery pipe is used to be connected to the capillary with a continuous phase; the collection side delivery pipe is used to be connected to the collection capillary; the generation side delivery pipe is used to be connected to the capillary with a dispersed phase; in addition, the ends of the four pipes away from the preparation cavity 5 are detachably connected to the plugs; the aforementioned generation side delivery pipe is connected to the generation nozzle 6, and the collection device is connected to the collection side delivery pipe. The following description will be made using the collection pipe 7 as an example of the collection device.

[0049] The 3D microemulsion preparation device provided in the present application provides a through hole 2 on the preparation body 1 and transparent windows at both ends of the through hole 2, so that the operator can intuitively observe the situation inside the preparation cavity 5, including the filling process of the continuous phase and the generation of microemulsions, thereby ensuring the accuracy of the operation and the consistency of the microemulsion quality. This visual design helps to adjust the operating parameters in a timely manner to ensure the stability of the preparation process and the quality of the product.

[0050] In the present application, four pipes are arranged on the preparation body 1, and the preparation cavity 5 is respectively adapted and connected to the continuous phase inlet capillary, the collection capillary and the dispersed phase inlet capillary through the pipes, and a top exhaust pipe is arranged. The structural design of the pipe and the preparation chamber is simple, and the liquid is directly introduced. Therefore, by adjusting the liquid flow rate of the pipe, the flow rate of the continuous phase and the dispersed phase can be effectively controlled and optimized, which simplifies the preparation process of the microemulsion droplets, and can ensure the sufficient mixing of the continuous phase and the dispersed phase, which helps to improve the preparation efficiency.

[0051] In this embodiment, see Figure 3 , the above-mentioned preparation body 1 can be a block structure, such as a square block structure, or a circular block structure. The above-mentioned through hole 2 is a through hole 2 opened at the center position of the preparation body 1. Along the length direction of the through hole 2, the two opposite side walls of the preparation body 1 are respectively provided with mounting grooves for installing a transparent window. The cross-sectional area of ​​the bottom of the mounting groove is larger than the cross-sectional area of ​​the through hole 2, and the bottom of the mounting groove is connected to the through hole 2. The above-mentioned transparent window mainly includes a glass plate 3 and a cover plate 4 covered on the glass plate 3. The glass plate 3 is embedded and installed in the mounting groove. An observation hole is opened at the center position of the cover plate 4. The cover plate 4 is located on the side of the glass plate 3 away from the through hole 2. The observation hole corresponds to the through hole 2 to facilitate the user to observe the situation in the preparation chamber. During specific installation, a plurality of fixing holes for installing screws can be set on the edge of the cover plate 4, and the cover plate 4 is detachably connected to the preparation body 1 by screws.

[0052] In this embodiment, the generation side conveying pipeline and the collection side conveying pipeline are arranged opposite to each other in the horizontal direction, and the generation nozzle 6 and the collection pipe 7 are arranged opposite to each other in the horizontal direction; the top exhaust pipeline and the feeding side conveying pipeline are arranged opposite to each other in the vertical direction, and the top exhaust pipeline is located above the feeding side conveying pipeline. Therefore, the four pipelines in this application are distributed in a cross shape.

[0053] The above-mentioned pipeline structure design combines the advantages of both co-flow (axisymmetric geometry) and flow focusing. Specifically: 1. In terms of optimizing flow symmetry: the generating nozzle and the collecting pipe are arranged in the horizontal direction, which helps to maintain the axisymmetry of the fluid flow. This arrangement is conducive to uniform mixing of the dispersed phase in the continuous phase and reduces the inconsistent droplet size caused by uneven flow; 2. In terms of improving the flow focusing effect: the top exhaust pipe is arranged above the feed side conveying pipe, which can effectively remove bubbles and control the flow direction of the fluid. This layout helps to optimize the flow focusing, so that the dispersed phase can be mixed with the continuous phase more accurately, thereby generating a more In terms of uniform microemulsion droplets; 3. In terms of reducing fluid resistance: horizontally arranged pipes can reduce the fluid resistance caused by pipe bends or corners, which helps to improve fluid delivery efficiency and preparation efficiency. The vertical exhaust pipe position helps to effectively remove bubbles in the system and maintain stable fluid flow in the system; 4. In terms of simplifying structural connections: this application arranges each pipe vertically and horizontally according to its function, which can effectively simplify the structural connection and make the assembly and maintenance of the equipment more convenient. The optimized design of the fluid flow path reduces pipe crossings and complex connection methods, which helps to improve the reliability and durability of the overall equipment.

[0054] In this embodiment, in order to adapt to different experimental conditions and requirements, the generation nozzle 6 in this application can be made of a variety of materials such as glass, ceramics and polymers, and the collection tube 7 can also be made of a variety of materials such as glass, ceramics and polymers, providing users with a wider range of choices. Of course, in specific applications, the material of the generation nozzle and the material of the collection device are adapted to the chemical solution used to prepare the microemulsion to ensure compatibility and performance. In the 3D microemulsion preparation device provided by this application, all liquid contact materials are made of stainless steel, ceramics and other materials, which have good corrosion resistance, solving the problem that materials such as PDMS, plastics, and glass used in traditional microfluidic chips cannot adapt to highly corrosive materials.

[0055] In this embodiment, the inner diameter of the generation nozzle ranges from 10 μm to 1 mm, and the inner diameter of the collection tube 7 or the collection nozzle ranges from 10 μm to 1 mm. Therefore, in this application, the inner and outer diameters of the generation nozzle 6 and the collection tube 7 are available in a variety of sizes, and users can flexibly combine them according to specific needs to achieve the best microemulsion droplet generation effect.

[0056] In this embodiment, a first connecting groove is formed at one end of the top exhaust pipe away from the preparation chamber 5, which is adapted to be plugged into the first plug 8; when filling the continuous phase, the first plug 8 is opened for exhaust, and the first plug 8 is installed in place after the continuous phase filling is completed.

[0057] In this embodiment, a second connecting groove is formed at the end of the feed-side delivery pipe distal from the preparation chamber 5, adapted to engage with the second plug 9. The second connecting groove is removably connected to the capillary tube carrying the continuous phase via a connector and a gasket. In one specific application example, the capillary tube carrying the continuous phase is connected to the second connecting groove via a 1 / 4-28 connector and a gasket. Of course, in other embodiments, an appropriate connector can be selected based on the specific dimensions of the second connecting groove.

[0058] In this embodiment, a production-side assembly groove 12 is provided on the side wall of the preparation body 1 where the production-side delivery pipe is provided. This production-side assembly groove 12 is a groove recessed inward from the side wall of the preparation body 1, and the bottom of the groove is connected to the production-side delivery pipe provided on the preparation body 1. A production-side plug 13 is adapted to be installed in this production-side assembly groove 12, and a production-side flow channel is provided on the production-side plug 13, which is connected to the production-side delivery pipe. Furthermore, a generation side baffle 14 is provided on the preparation body 1, and the generation side baffle 14 is detachably connected to the preparation body 1 by screws. The generation side baffle 14 can encapsulate the generation side plug 13 in the generation side assembly groove 12. The generation side baffle 14 is provided with a baffle channel corresponding to the generation side flow channel, and the baffle channel is detachably connected to the third plug 10; a sealing groove is provided on the side wall where the generation side plug 13 and the generation side baffle 14 are connected, and a sealing ring 17 is provided in the sealing groove, and the end of the baffle channel connected to the generation side flow channel abuts against the sealing ring.

[0059] This application provides a sealing groove and a sealing ring on the side wall where the generation-side plug 13 and the generation-side baffle 14 meet, effectively preventing fluid leakage and ensuring a tight seal between the generation-side flow channel and the generation-side delivery pipeline. This sealing design reduces the risk of fluid leakage during delivery and improves the reliability and stability of the equipment.

[0060] The production side baffle 14 is detachably connected to the preparation body 1 via screws. This design allows for easy removal and maintenance of the production side plug 13 and its associated components. Maintenance personnel can quickly remove the baffle to conduct necessary inspections or replace the production side plug 13 without disassembling the entire device, improving maintenance efficiency.

[0061] The connection method of the generating side assembly groove 12, the generating side plug 13 and the generating side delivery pipe of the present application allows the plug to be accurately installed in the groove and kept stable by the encapsulation of the baffle. This structural design simplifies the installation process of the plug and improves the assembly accuracy and consistency.

[0062] The side baffle 14 of the present invention encapsulates the side plug 13, effectively fixing the plug's position and reducing displacement caused by vibration or external forces. This stable structure helps maintain the flow direction of the flow channel, thereby improving the operating stability of the device and the uniformity of the fluid flow.

[0063] In the present application, the connection between the generation side flow channel on the generation side plug 13 and the generation side delivery pipeline is more precise, so that the fluid can be distributed into the flow channel in a more uniform manner. This optimization can improve the uniformity and stability of the microemulsion droplets.

[0064] In the present application, different generation side plugs 13 and collection side plugs 15 can be disassembled and replaced, so that users can easily prepare microemulsions with complex structures such as double emulsions.

[0065] The following are several optimization methods that allow users to prepare microemulsion droplets with complex structures through optimization in the following aspects:

[0066] 1. Adjust the flow channel configuration: By replacing different generation side plugs 13 and collection side plugs 15, it is possible to adapt to replacing generation nozzles 6 and collection tubes 7 or collection nozzles of different geometric shapes and sizes, thereby controlling the shape and size of microemulsion droplets. In this way, users can adjust the fluid distribution method as needed to achieve different droplet structures and sizes.

[0067] 2. Changing the fluid contact angle: The generation side plugs 13 and baffles with different structures can be made to change the contact angle and flow rate of the fluid in the flow channel, affecting the formation mode of the emulsion droplets, so that complex structures such as double emulsion droplets can be realized.

[0068] In this embodiment, a collection-side assembly groove is provided on the side wall of the preparation body 1, where the collection-side delivery pipe is provided. This collection-side assembly groove is a groove recessed inward from the side wall of the preparation body 1, and the bottom of the groove is connected to the collection-side delivery pipe provided on the preparation body 1. A collection-side plug 15 is adapted to be installed in this collection-side assembly groove, and the collection-side plug 15 defines a collection-side flow channel, which is connected to the collection-side delivery pipe. Furthermore, a collecting side baffle 16 is provided on the preparation body 1, and the collecting side baffle 16 is detachably connected to the preparation body 1 by screws. The collecting side baffle 16 can encapsulate the collecting side plug 15 in the collecting side assembly groove. The collecting side baffle 16 is provided with a baffle channel corresponding to the collecting side flow channel, and the baffle channel is detachably connected to the third plug 10; a sealing groove is provided on the side wall where the collecting side plug 15 and the collecting side baffle 16 are connected, and a sealing ring is provided in the sealing groove, and the end of the baffle channel connected to the collecting side flow channel abuts against the sealing ring.

[0069] This application provides a sealing groove and a sealing ring on the side wall where the collection-side plug 15 and the collection-side baffle 16 meet, effectively preventing fluid leakage and ensuring a tight seal between the collection-side flow channel and the collection-side delivery pipeline. This sealing design reduces the risk of fluid leakage during delivery and improves the reliability and stability of the equipment.

[0070] The collection-side baffle 16 of the present application is detachably connected to the preparation body 1 via screws. This design allows for easy removal and maintenance of the collection-side plug 15 and its associated components. Maintenance personnel can quickly remove the baffle to conduct necessary inspections or replace the collection-side plug 15 without disassembling the entire device, improving maintenance efficiency.

[0071] The connection method of the collection side assembly groove, the collection side plug 15 and the collection side delivery pipe of the present application allows the plug to be accurately installed in the groove and maintained stable by the encapsulation of the baffle. This structural design simplifies the installation process of the plug and improves assembly accuracy and consistency.

[0072] The collector side baffle 16 of the present application encapsulates the collector side plug 15, effectively securing the plug's position and reducing displacement caused by vibration or external forces. This stable structure helps maintain the flow direction of the flow channel, thereby improving the operating stability of the device and the uniformity of the fluid flow.

[0073] Compared with traditional 2D microfluidic chips, in the 3D microemulsion preparation device provided by the present application, the generation nozzle and the collection tube or the collection nozzle are suspended in the preparation cavity and a spacing is left in the middle according to the design (the installation spacing range is 10μm to 500μm), so that the microemulsions are in a 3D free sphere state during generation and collection, which is conducive to the generation of microemulsions, solves the problem that some solutions cannot pass through the microfluidic chip and cannot generate microemulsions, and ensures the stability of the microemulsions. The generation frequency of microemulsions is significantly improved compared with the generation frequency of ordinary chips; furthermore, the 3D microemulsion preparation device provided by the present application uses standard microfluidic connectors (1 / 4-28 or 10-1 / 32) and standard capillaries (1 / 16 inch or 1 / 32 inch), using a straight line connection in the same direction, which is simple to connect, has good sealing, and ensures good repeatability of the preparation; this solves the problem of difficult connection and leakage between traditional 2D microfluidic chips and capillaries, and more importantly, solves the problem of microemulsion fusion or rupture caused by the vertical connection method commonly used in traditional 2D microfluidic chips. Furthermore, the internal structural design of the 3D microemulsion preparation device provided by this application simultaneously features co-flow (axisymmetric geometry) and flow focusing, eliminating the need for internal coatings and surface modifications, and simplifying the preparation process. Furthermore, each component of the 3D microemulsion preparation device provided by this application is disassembled, making it easy to assemble and disassemble, clean, and reuse. Furthermore, the materials of the generating nozzle 6 and the collecting device in the present application are optional, such as glass, ceramics and polymers, which can be adapted to various types of reagents, including relatively viscous reagents or corrosive reagents. The material selection of the generating nozzle 6 and the collecting tube 7 is conducive to improving its high temperature resistance and corrosion resistance. The material of the sealing ring in the present application should also be selected to have high temperature resistance and corrosion resistance, such as fluororubber, silicone rubber, polytetrafluoroethylene and other materials; on this basis, the inner and outer diameters of the generating nozzle 6 and the collecting tube 7 in the present application are optional, and various combinations can be made to generate microemulsions of different sizes. The specific material and size of the generating nozzle 6 and the collecting tube 7 can be configured according to experimental requirements; in addition, the present application can prepare microemulsions with complex structures such as double emulsions by disassembling and replacing the plug and baffle on the left generating side.

[0074] Therefore, the microemulsion preparation device provided in the present application has a simple structure, low manufacturing, use and maintenance costs, a transparent window is provided for easy observation of the preparation process, and is easy to operate and use.

[0075] Example 2

[0076] The present invention provides a method for preparing microemulsion droplets, which is prepared using the 3D microemulsion preparation device described in the above embodiment 1. The specific preparation method is as follows, see Figure 1 :

[0077] 1. Remove the plugs above, below, and on the collection side of the preparation chamber;

[0078] 2. Connect the capillary tube with the continuous phase to the bottom of the cavity through a 1 / 4-28 joint and a gasket; connect one end of the collection capillary tube to the collection side of the preparation body through a 1 / 4-28 joint and a gasket, and place the other end into the collection container;

[0079] 3. Place the preparation body vertically with the top exhaust pipe facing upwards. Pass the continuous phase into the preparation chamber at a high flow rate and observe the filling process through the glass window. If bubbles are generated, gently shake the device to expel them. When the chamber is full of continuous phase, plug the top exhaust pipe with a plug and reduce the continuous phase flow rate.

[0080] 4. Remove the plug installed on the generation side of the preparation body, connect the capillary containing the dispersed phase to the generation side through a 1 / 4-28 joint and a gasket, and introduce the dispersed phase into the preparation cavity at the target flow rate to generate microemulsion droplets of target size and target frequency distribution in the preparation cavity. The generated microemulsion droplets are sent to the collection container through the collection tube in the preparation cavity.

[0081] In the microemulsion preparation method provided in the present application, microemulsions of different sizes and different frequency distributions can be generated by adjusting the flow rates of the dispersed phase and the continuous phase.

[0082] During the preparation process, microemulsion droplets may form droplets of different sizes, depending on factors such as the ratio of the ingredients, the mixing method and conditions. For example, the size of microemulsion droplets can range from nanometers to micrometers. Therefore, in this application, the frequency distribution of microemulsion droplets can be understood as the frequency of occurrence of microemulsion droplets of different sizes in the overall liquid. In other words, microemulsion droplets of certain sizes may be more common, while microemulsion droplets of other sizes are less common.

[0083] It can be seen that the use of the 3D microemulsion preparation device provided in the present application to prepare microemulsions can simplify the operating process. When in use, microemulsions of different sizes and different frequency distributions can be generated by adjusting the flow rate of the dispersed phase and / or the flow rate of the continuous phase introduced into the preparation cavity. This flexible adjustment capability enables the device to meet different application requirements, thereby improving the applicability and flexibility of the 3D microemulsion preparation device. Therefore, the use of the 3D microemulsion preparation device provided in the present application can reduce preparation costs and simplify the preparation process.

[0084] The 3D microemulsion preparation device provided by the present application is also easy to clean. For example, when cleaning the generating nozzle, the upper part of the cavity and the collecting side can be blocked with a plug, and a cleaning liquid is introduced from the bottom of the cavity so that it flows out from the generating side, and the generating nozzle is reversely flushed. In most cases, this method can flush out the blockage. If it cannot be flushed out, the generating nozzle can be removed and ultrasonically cleaned. When cleaning the preparation cavity, the transparent window can be removed from the preparation body, and then the preparation cavity can be flushed with a flushing liquid. Therefore, the 3D microemulsion preparation device provided by the present application has a simple structure, is easy to operate and use, has a simple cleaning operation, and has low manufacturing, use and maintenance costs. In addition, the use of the device can simplify the preparation process of microemulsions and reduce the difficulty of the preparation operation.

[0085] The technical features of the above embodiments can be combined arbitrarily (as long as there is no contradiction in the combination of these technical features). In order to make the description concise, not all possible combinations of the technical features in the above embodiments are described; these embodiments that are not explicitly written should also be considered to be within the scope of this specification.

[0086] The present application has been described in a relatively specific and detailed manner through general explanations and specific embodiments. It should be understood that, based on the technical concept of the present application, several conventional adjustments or further innovations may be made to these specific embodiments; however, as long as they do not depart from the technical concept of the present application, the technical solutions obtained by such conventional adjustments or further innovations also fall within the scope of protection of the claims of the present application.

Claims

1. A 3D microemulsion preparation device, characterized in that: The preparation device comprises a preparation body, wherein a through hole is formed on the preparation body, transparent windows are installed at both ends of the through hole, the channel of the through hole and the two transparent windows together form a preparation cavity, and a generation nozzle and a collection device arranged opposite to the generation nozzle are provided in the preparation cavity, wherein the collection device is a collection tube or a collection nozzle; The preparation body is provided with a top exhaust pipe, a feed side delivery pipe adapted to be connected to a capillary tube through which a continuous phase passes, a collection side delivery pipe adapted to be connected to a collection capillary tube, and a generation side delivery pipe adapted to be connected to a capillary tube through which a dispersed phase passes; the top exhaust pipe, the feed side delivery pipe, the collection side delivery pipe and the generation side delivery pipe are respectively connected to the preparation chamber, the generation side delivery pipe is connected to the generation nozzle, and the collection device is connected to the collection side delivery pipe; the top exhaust pipe, the feed side delivery pipe, the collection side delivery pipe and the generation side delivery pipe are respectively detachably connected to a plug at one end away from the preparation chamber; The preparation body is a block structure, the through hole is a through hole opened at the center of the preparation body, and along the length direction of the through hole, two opposite side walls of the preparation body are respectively provided with mounting grooves for mounting the transparent window, the cross-sectional area of ​​the bottom of the mounting groove is larger than the cross-sectional area of ​​the through hole, and the bottom of the mounting groove is connected to the through hole; The generation side conveying pipe and the collection side conveying pipe are arranged opposite to each other in the horizontal direction, and the generation nozzle and the collection pipe or the collection nozzle are arranged opposite to each other in the horizontal direction; the top exhaust pipe and the feed side conveying pipe are arranged opposite to each other in the vertical direction, and the top exhaust pipe is located above the feed side conveying pipe; A generation side assembly groove is provided on the side wall of the preparation body on which the generation side delivery pipeline is provided, a generation side plug is adapted to be installed in the generation side assembly groove, a generation side flow channel is provided on the generation side plug, and the generation side flow channel is communicated with the generation side delivery pipeline; a generation side baffle is provided on the preparation body, the generation side baffle is detachably connected to the preparation body by screws, the generation side baffle can encapsulate the generation side plug in the generation side assembly groove, a baffle channel corresponding to the generation side flow channel is provided on the generation side baffle, and the baffle channel is detachably connected to the third plug; A sealing groove is provided on the side wall where the generation side plug and the generation side baffle meet, a sealing ring is provided in the sealing groove, and one end of the baffle channel where the baffle channel meets the generation side flow channel abuts against the sealing ring; A collecting side assembly groove is provided on the side wall of the preparation body on which the collecting side delivery pipe is provided, a collecting side plug is adapted to be installed in the collecting side assembly groove, a collecting side flow channel is provided on the collecting side plug, and the collecting side flow channel is communicated with the collecting side delivery pipe; a collecting side baffle is provided on the preparation body, the collecting side baffle is detachably connected to the preparation body by screws, the collecting side baffle can encapsulate the collecting side plug in the collecting side assembly groove, a baffle channel corresponding to the collecting side flow channel is provided on the collecting side baffle, and the baffle channel is detachably connected to the fourth plug; A sealing groove is provided on the side wall where the collecting side plug is connected to the collecting side baffle. A sealing ring is provided in the sealing groove. One end of the baffle channel connected to the collecting side flow channel abuts against the sealing ring.

2. The 3D microemulsion preparation device according to claim 1, characterized in that: The transparent window includes a glass plate and a cover plate covered on the glass plate. The glass plate is embedded in the mounting groove. An observation hole is provided at the center of the cover plate. The cover plate is located on the side of the glass plate away from the through hole. The observation hole corresponds to the through hole. A plurality of fixing holes for installing screws are provided on the edge of the cover plate. The cover plate is detachably connected to the preparation body by screws.

3. The 3D microemulsion preparation device according to claim 1, characterized in that: An end of the top exhaust pipe away from the preparation chamber forms a first connecting groove adapted to be plugged into a first plug; The end of the feeding side delivery pipe away from the preparation chamber forms a second connecting groove adapted to be plugged with a second plug, and the second connecting groove is detachably connected to the capillary tube through which the continuous phase passes through a connecting joint and a gasket.

4. The 3D microemulsion preparation device according to claim 1, characterized in that The materials of the generating nozzle and the collecting device are adapted to the chemical solution used to prepare the microemulsion droplets to ensure compatibility and performance; The material of the generating nozzle is glass, polymer material, ceramic or metal, and the inner diameter of the generating nozzle ranges from 10 μm to 1 mm; The material of the collecting tube or collecting nozzle is glass, polymer material, ceramic or metal, and the inner diameter of the collecting tube or collecting nozzle ranges from 10 μm to 1 mm; The installation distance between the generating nozzle and the collecting device ranges from 10 μm to 500 μm.

5. A method for preparing microemulsion droplets, characterized in that: The 3D microemulsion preparation device according to any one of claims 1 to 4 is used, and the microemulsion preparation method comprises the following steps: S1: Remove all the plugs installed on the top exhaust pipe, the feeding side conveying pipe and the collecting side conveying pipe; S2: fixedly connecting the capillary tube with the continuous phase to the feeding side delivery pipe, fixedly connecting one end of the collecting capillary tube to the collecting side delivery pipe, and connecting the other end of the collecting capillary tube to the collection container; S3: The preparation body is placed vertically so that the top exhaust pipe is above the preparation cavity, and the continuous phase is introduced into the preparation cavity at a target flow rate. The filling process of the continuous phase in the preparation cavity is observed through a transparent window. When the preparation cavity is full of the continuous phase, the top exhaust pipe is blocked with a plug, and the flow rate of the continuous phase is reduced. S4: Remove the plug installed on the generation side delivery pipeline, fix the capillary tube with the dispersed phase to the generation side delivery pipeline, introduce the dispersed phase into the preparation cavity at a target flow rate, generate microemulsion droplets of target size and target frequency distribution in the preparation cavity, and deliver the generated microemulsion droplets to the collection container through the collection tube in the preparation cavity.

6. The method for preparing microemulsion droplets according to claim 5, characterized in that: In step S3, if bubbles are generated during the filling process of the continuous phase, the preparation body is gently shaken to allow the air in the preparation body to be discharged from the top exhaust pipe to eliminate the bubbles; In the microemulsion preparation method, microemulsions of different sizes and different frequency distributions are generated by adjusting the flow rate of the dispersed phase and / or the flow rate of the continuous phase introduced into the preparation cavity.

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