3D microemulsion droplet preparation device and preparation method

Abstract

The invention discloses a 3D micro-emulsion droplet preparation device and method.The 3D micro-emulsion droplet preparation device comprises a preparation cavity formed in a preparation body, transparent windows are arranged on the front side and the rear side of the preparation cavity, and a top exhaust pipeline, a feeding side conveying pipeline, a collecting side conveying pipeline and a generating side conveying pipeline are arranged on the preparation body; the four pipelines communicate with the preparation cavity, and the ends, away from the preparation cavity, of the four pipelines are detachably connected with the plugs correspondingly. During use, the preparation body is vertically placed, plugs above and below the preparation cavity and on the collection side are removed, a continuous phase is introduced into the preparation cavity through the feeding side conveying pipeline, the exhaust pipeline at the top is blocked after the preparation cavity is filled with the continuous phase, the plug installed on the generation side conveying pipeline is removed, and a dispersed phase is introduced through the generation side conveying pipeline. The micro-emulsion droplets with different sizes and frequencies can be prepared by adjusting the flow rates of the dispersed phase and the continuous phase, the whole structure is simple and clear, observation is convenient, operation and use are simple, the preparation cost can be reduced, and the preparation process is simplified.

Description

Technical Field

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

[0002] Microemulsion droplets are a liquid system with a special structure, in which oil, water and surfactants (some also have co-surfactants) form stable droplets under specific conditions. These droplets have nanometer or micrometer sizes and can be evenly dispersed in mixed solvents. Microemulsions have many advantages, such as high specific surface area, high-throughput processing, independent reaction chambers, rapid mixing and heat transfer effects, and can be used as microreactors, etc.

[0003] The preparation methods of microemulsions mainly include early high-speed stirring, layer-by-layer assembly technology, membrane emulsification 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 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 method. 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 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 a preparation method thereof. This document is based on the microfluidic system to prepare microemulsions.

[0004] Although microemulsions can be prepared by the above-mentioned preparation methods, the above-mentioned preparation methods still have the following defects in actual production: Although the early preparation methods are simple to operate, the uniformity of the generated microemulsions 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 the microfluidic system 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, a groove is engraved on one of the plates, and then bonded (glued) to the other plate. The traditional 2D microfluidic chip is affected by the material properties of the inner wall of the chip microchannel, and many solutions cannot interact to generate microemulsions; 2) Existing microfluidic chips have problems such as easy clogging, difficult to clean, slow generation rate, and difficulty in generating multiple emulsions; 3) Microfluidic chips need to perform complex surface modification (hydrophilic and hydrophobic modification) according to the different types of microemulsion structures; In short, the preparation cost of microemulsions is high and the preparation process is complicated. Therefore, the current preparation cost of microemulsion is high, the preparation process is complicated, and many solutions cannot generate microemulsions through the principle of microfluidic chips. Therefore, it is necessary to propose a new technical solution to solve the problems existing in the prior art. Summary of the invention

[0005] The present application provides a 3D microemulsion preparation device and preparation method, which are used 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 provided on the preparation body, 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, a generation nozzle and a collecting device arranged opposite to the generation nozzle are arranged in the preparation cavity, and the collecting device is a collecting tube or a collecting nozzle; a top exhaust pipe, a feeding side delivery pipe for being adapted and connected to a capillary through which a continuous phase passes, a collecting side delivery pipe for being adapted and connected to a collecting capillary, and a generation side delivery pipe for being adapted and connected to a capillary through which a dispersed phase passes are arranged 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 a 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, 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 mounting 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 arranged 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 adapted to be plugged into the first plug is formed at one end of the top exhaust pipe away from the preparation chamber; a second connecting groove adapted to be plugged into the second plug is formed at one end of the feed side delivery pipe away from the preparation chamber, and the second connecting groove is detachably connected to the capillary tube passing the continuous phase 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 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 is connected to the generation side baffle, a sealing ring is provided in the sealing groove, and one 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 pipeline 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 with the collecting side conveying pipeline; 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 one 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 compatible with the chemical solution used to prepare the microemulsion droplets to ensure compatibility and performance.

[0015] Furthermore, the material of the generated nozzle is glass, polymer material, ceramic or metal, and the inner diameter size range of the generated nozzle is 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 spacing 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, and the method for preparing microemulsion droplets comprises the following steps:

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

[0020] S2: The capillary tube through which the continuous phase passes is fixedly connected to the delivery pipeline on the feeding side, one end of the collecting capillary tube is fixedly connected to the delivery pipeline on the collecting side, and the other end of the collecting capillary tube is connected to the collecting container;

[0021] S3: Place the preparation body vertically so that the top exhaust pipe is above the preparation cavity, pass the continuous phase into the preparation cavity at a target flow rate, and observe the filling process of the continuous phase in the preparation cavity through a transparent window. When the preparation cavity 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 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 so that the air in the preparation body is discharged from the top exhaust pipe to eliminate the bubbles.

[0024] Furthermore, in the above-mentioned method for preparing microemulsion droplets, microemulsion droplets of different sizes and different frequency distributions are generated by adjusting the flow rate of the dispersed phase introduced into the preparation cavity 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; the use of the device to prepare microemulsions can simplify the operation 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 passed into the preparation cavity and / or the flow rate of the continuous phase passed 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, the use of the microemulsion preparation device provided in the present application can reduce the preparation cost and simplify the preparation process.

[0027] 2. The 3D microemulsion preparation device provided in the present 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 is convenient to install and use, and the microemulsion preparation operation is simple.

[0029] 4. When using the 3D microemulsion preparation device to prepare microemulsions, 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 a continuous phase is connected to the feeding side delivery pipe, the collecting capillary and the collecting 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 a 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 collecting container through the collecting pipe in the preparation cavity. It can be seen that the device is easy to operate and use, and the microemulsion preparation process is concise.

[0030] 5. In the 3D microemulsion preparation device provided in the present application, the generating nozzle and the collecting tube or the collecting 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 PDMS, plastic, glass and other materials used in traditional microfluidic chips cannot be adapted to highly corrosive materials.

[0032] 7. The 3D microemulsion preparation device provided in the present application adopts a modular design and consists of a preparation chamber, 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 the present application adopts a standard microfluidic connector (1 / 4-28 or 10-1 / 32) and a standard capillary (1 / 16 inch or 1 / 32 inch), and adopts 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 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 is a brief introduction to 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 usually be regarded as limiting conditions for implementing the present application; for example, based on the technical concepts and exemplary drawings disclosed in the present application, those skilled in the art are able to easily make routine adjustments or further optimizations to the increase / decrease / 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 an 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 an embodiment;

[0038] Figure 4 for Figure 1 A schematic diagram of the front view 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 A 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. Collect the pipe; 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. Collect the side plug; 16. Collect the side baffle; 17. Sealing ring;

[0043] A. Top exhaust pipe; B. Delivery pipe on the feeding side; C. Delivery pipe on the collecting side; D. Delivery pipe on the generating side. DETAILED DESCRIPTION

[0044] The present application is 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 special meanings in terms of technical connotations (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] The terms such as "upper", "lower", "left", "right", "middle", etc. used in this application are usually used to facilitate intuitive understanding by comparing with the accompanying drawings, and are not absolute limitations on the positional relationship in the actual product. Without departing from the technical concept disclosed in this application, changes in these relative positional relationships should also be regarded as the scope of this application.

[0047] Embodiment 1

[0048] The present application provides a 3D microemulsion preparation device, see Figure 1 , 2 , mainly including a preparation body 1, which is the structural installation foundation of the device. Specifically, a through hole 2 is provided on the preparation body 1, and transparent windows are installed at both ends of the through hole 2 respectively. The channel of the through hole 2 and the two transparent windows together form a preparation cavity 5, which is the microemulsion droplet generation cavity of the device. A generation nozzle 6 and a collection device arranged opposite to the generation nozzle 6 are arranged in the preparation cavity 5, and the collection device is a collection tube or a collection nozzle. The preparation body 1 is also provided with four pipes, which are connected to the preparation cavity 5 respectively, and the feeding, exhaust, microemulsion generation and microemulsion collection are realized 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 arranged at the top of the preparation body 1 to realize the exhaust of gas in the cavity during feeding; the feeding side delivery pipe is used to be connected with the capillary through which the continuous phase passes; the collection side delivery pipe is used to be connected with the collection capillary; the generation side delivery pipe is used to be connected with the capillary through which the dispersed phase passes; in addition, the ends of the four pipes away from the preparation cavity 5 are detachably connected with the plugs respectively; and the aforementioned generation side delivery pipe is connected with the generation nozzle 6, and the collection device is connected with the collection side delivery pipe. The following is an example of the collection device using the collection pipe 7.

[0049] The 3D microemulsion preparation device provided in the present application, by setting a through hole 2 on the preparation body 1 and setting transparent windows at both ends of the through hole 2, allows the operator to intuitively observe the situation in 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 quality of the microemulsions. This visual design helps to adjust the operating parameters in time 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 connected with the continuous phase inlet capillary, the collecting 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, the flow rate of the continuous phase and the dispersed phase can be effectively controlled and optimized by adjusting the liquid flow rate of the pipe, which simplifies the preparation process of the microemulsion droplets, ensures the full mixing of the continuous phase and the dispersed phase, and 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 greater 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 pipeline structure design combines the advantages of co-flow (axisymmetric geometry) and flow focusing. Specifically: 1. In terms of optimizing flow symmetry: the generating nozzle and the collecting tube 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 inconsistency of droplet size caused by uneven flow; 2. In terms of improving the flow focusing effect: the top exhaust pipe is arranged above the conveying pipe on the feeding side, 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 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 crossing 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 generating nozzle 6 in this application can be made of various materials such as glass, ceramics and polymers, and the collecting tube 7 can also be made of various materials such as glass, ceramics and polymers, providing users with a wider range of choices. Of course, in specific applications, 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. 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 the 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 generating nozzle is in the range of 10 μm to 1 mm, and the inner diameter of the collecting tube 7 or the collecting nozzle is in the range of 10 μm to 1 mm. Therefore, in this application, the inner and outer diameters of the generating nozzle 6 and the collecting tube 7 have a variety of optional specifications, 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 adapted to be plugged into the first plug 8 is formed at one end of the top exhaust pipe away from the preparation chamber 5; 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 is filled.

[0057] In this embodiment, the end of the feeding side delivery pipeline away from the preparation chamber 5 forms a second connection groove adapted to be plugged with the second plug 9, and the second connection groove is detachably connected to the capillary tube with the continuous phase through a connection joint and a gasket. In a specific application example, the capillary tube with the continuous phase can be connected to the second connection groove through a 1 / 4-28 joint and a gasket. Of course, in other embodiments, a suitable connection joint can be selected according to the specific size of the second connection groove.

[0058] In this embodiment, a generation side assembly groove 12 is provided on the side wall of the preparation body 1 on which the generation side delivery pipeline is provided. The generation side assembly groove 12 is a groove that is recessed inward from the side wall of the preparation body 1, and the bottom of the groove is connected to the generation side delivery pipeline provided on the preparation body 1. A generation side plug 13 is adapted and installed in the generation side assembly groove 12, and a generation side flow channel is provided on the generation side plug 13, and the generation side flow channel is connected to the generation side delivery pipeline. 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, and a baffle channel corresponding to the generation side flow channel is opened on the generation side baffle 14, and the baffle channel is detachably connected to the third plug 10; a sealing groove is opened on the side wall where the generation side plug 13 and the generation side baffle 14 are connected, and a sealing ring 17 is arranged in the sealing groove, and the end of the baffle channel connected to the generation side flow channel abuts against the sealing ring.

[0059] The present application provides a sealing groove on the side wall where the generation side plug 13 and the generation side baffle 14 meet, and is equipped with a sealing ring, which can effectively prevent fluid leakage and ensure the sealing between the generation side flow channel and the generation side delivery pipeline. This sealing design reduces the risk of fluid leakage during the delivery process and improves the reliability and stability of the equipment.

[0060] The side baffle plate 14 of the present application is detachably connected to the preparation body 1 by screws, and this design allows the side plug 13 and its related components to be easily disassembled and maintained. Maintenance personnel can quickly disassemble the baffle plate and conduct necessary inspections or replace the side plug 13 without disassembling the entire device, thereby improving maintenance efficiency.

[0061] The connection method between 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 maintained stable by the encapsulation of the baffle. This structural design simplifies the installation process of the plug and improves assembly accuracy and consistency.

[0062] The generated side baffle 14 of the present application encapsulates the generated side plug 13, which can effectively fix the position of the plug and reduce the displacement caused by vibration or external force. This stable structure helps to keep the flow direction of the flow channel unchanged, thereby improving the working stability of the equipment and the uniformity of 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] Several optimization methods are provided below, so that users can prepare microemulsion droplets with complex structures by optimizing the following aspects:

[0066] 1. Adjust the flow channel configuration: Replace different generation side plugs 13 and collection side plugs 15 to adapt to the replacement of generation nozzles 6 and collection tubes 7 or collection nozzles of different geometric shapes and sizes, thereby controlling the shape and size of micro-emulsion 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, affect the formation mode of the emulsion droplets, and realize complex structures such as double emulsion droplets.

[0068] In this embodiment, a collecting side assembly groove is provided on the side wall of the preparation body 1 on which the collecting side delivery pipeline is provided. The collecting side assembly groove is a groove that is recessed inward from the side wall of the preparation body 1, and the bottom of the groove is connected to the collecting side delivery pipeline provided on the preparation body 1. A collecting side plug 15 is adapted and installed in the collecting side assembly groove, and a collecting side flow channel is provided on the collecting side plug 15, and the collecting side flow channel is connected to the collecting side delivery pipeline. 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] The present application provides a sealing groove on the side wall where the collecting side plug 15 and the collecting side baffle 16 meet, and is equipped with a sealing ring, which can effectively prevent fluid leakage and ensure the sealing between the collecting side flow channel and the collecting side delivery pipeline. This sealing design reduces the risk of fluid leakage during the delivery process and improves the reliability and stability of the equipment.

[0070] The collecting side baffle 16 of the present application is detachably connected to the preparation body 1 by screws, and this design allows the collecting side plug 15 and its related components to be easily disassembled and maintained. Maintenance personnel can quickly disassemble the baffle and conduct necessary inspections or replace the collecting side plug 15 without disassembling the entire device, thereby improving maintenance efficiency.

[0071] The connection method between the collection side assembly groove, the collection side plug 15 and the collection side delivery pipeline 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 collecting side baffle 16 of the present application encapsulates the collecting side plug 15, which can effectively fix the position of the plug and reduce the displacement caused by vibration or external force. This stable structure helps to keep the flow direction of the flow channel unchanged, thereby improving the working stability of the equipment and the uniformity of fluid flow.

[0073] Compared with the traditional 2D microfluidic chip, in the 3D microemulsion preparation device provided by the present application, the generating nozzle and the collecting tube or the collecting 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 microemulsion is in a 3D free sphere state during the 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; further, the 3D microemulsion preparation device provided by the present application adopts a standard microfluidic connector (1 / 4-28 or 10-1 / 32) and a standard capillary (1 / 16 inch or 1 / 32 inch), and adopts 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 the traditional 2D 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 the traditional 2D microfluidic chip. Furthermore, the internal structure design of the 3D microemulsion preparation device provided by the present application has the characteristics of co-flow (axisymmetric geometry) and flow focusing, avoiding the problem of internal coating and surface modification, and simplifying the preparation operation process. In addition, each component of the 3D microemulsion preparation device provided by the present application can be disassembled, and the overall assembly and disassembly are convenient, easy to clean and reusable. Furthermore, the materials of the generating nozzle 6 and the collecting device in the present application include glass, ceramics, polymers, etc., 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 with 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 to facilitate observation of the preparation process, and is easy to operate and use.

[0075] Embodiment 2

[0076] The present application 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 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 relatively high flow rate, and observe the filling process through the glass window; if bubbles are generated, gently shake the device to expel the bubbles; when the chamber is filled with the continuous phase, plug the top exhaust pipe with a plug and reduce the flow rate of the continuous phase;

[0080] 4. Remove the plug installed on the generation side of the preparation body, connect the capillary with 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 a 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 method for preparing microemulsion droplets provided in the present application, microemulsion droplets of different sizes and different frequency distributions can be generated by adjusting the flow rates of the dispersed phase and the continuous phase.

[0082] Microemulsion droplets may form droplets of different sizes during the preparation process, depending on the ratio of the components, the mixing method and conditions, etc. For example, the size of the microemulsion droplets can vary from nanometers to micrometers, so the microemulsion droplets with different frequency distributions in this application can be understood as the frequency of occurrence of microemulsion droplets of different sizes in the overall liquid, that is, 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 operation process. When in use, microemulsions of different sizes and different frequency distributions can be generated by adjusting the flow rate of the dispersed phase passed into the preparation cavity and / or the flow rate of the continuous phase passed 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 to make it flow out from the generating side, and the generating nozzle is backwashed. In most cases, this method can flush out the blockage. If it cannot be flushed out, the generating nozzle can be removed and cleaned ultrasonically; when cleaning the preparing cavity, the transparent window can be removed from the preparing body, and then the preparing 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, has a low cost of manufacturing, using and maintaining the device, and can simplify the preparation process of microemulsions and reduce the difficulty of preparation operations.

[0085] The technical features of the above embodiments may be arbitrarily combined (as long as there is no contradiction in the combination of these technical features). 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 above is a relatively specific and detailed description of the present application through general description and specific embodiments. It should be understood that, based on the technical concept of the present application, several conventional adjustments or further innovations can be made to these specific embodiments; however, as long as they do not deviate from the technical concept of the present application, the technical solutions obtained by these 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, It is characterized in that The preparation body comprises a through hole, the through hole is provided with transparent windows at both ends of the through hole, the through hole and the two transparent windows together form a preparation cavity, a generating nozzle and a collecting device arranged opposite to the generating nozzle are arranged in the preparation cavity, and the collecting device is a collecting tube or a collecting nozzle; The preparation body is provided with a top exhaust pipe, a feed side delivery pipe for being connected to a capillary through which a continuous phase passes, a collection side delivery pipe for being connected to a collection capillary, and a generation side delivery pipe for being connected to a capillary 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 cavity, 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 cavity.

2. The 3D microemulsion preparation device according to claim 1, It is characterized in that 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, 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.

3. The 3D microemulsion preparation device according to claim 2, It is 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, and the cover plate is detachably connected to the preparation body by screws.

4. The 3D microemulsion preparation device according to claim 1, It is characterized in that 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 and the collection pipe or the collection 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.

5. The 3D microemulsion preparation device according to claim 4, It is characterized in that One end of the top exhaust pipe away from the preparation chamber forms a first connecting groove adapted to be plugged with a first plug; The end of the feeding side delivery pipeline 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 a capillary tube having a continuous phase through a connecting joint and a gasket.

6. The 3D microemulsion preparation device according to claim 4, It is characterized in that A generating side assembly groove is arranged on the side wall of the preparation body on which the generating side delivery pipeline is arranged, a generating side plug is adapted and installed in the generating side assembly groove, a generating side flow channel is arranged on the generating side plug, and the generating side flow channel is communicated with the generating side delivery pipeline; a generating side baffle is arranged on the preparation body, the generating side baffle is detachably connected to the preparation body by screws, the generating side baffle can encapsulate the generating side plug in the generating side assembly groove, a baffle channel corresponding to the generating side flow channel is arranged on the generating side baffle, and the baffle channel is detachably connected to the third plug; A sealing groove is provided on the side wall where the generating side plug is connected to the generating side baffle, a sealing ring is arranged in the sealing groove, and one end of the baffle channel connected to the generating side flow channel abuts against the sealing ring.

7. The 3D microemulsion preparation device according to claim 4, It is characterized in that The side wall of the preparation body on which the collection side delivery pipeline is provided is provided with a collection side assembly groove, a collection side plug is adapted and installed in the collection side assembly groove, a collection side flow channel is provided on the collection side plug, and the collection side flow channel is communicated with the collection side delivery pipeline; a collection side baffle is provided on the preparation body, the collection side baffle is detachably connected to the preparation body by screws, the collection side baffle can encapsulate the collection side plug in the collection side assembly groove, a baffle channel corresponding to the collection side flow channel is provided on the collection 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 arranged in the sealing groove, and one end of the baffle channel connected to the collecting side flow channel abuts against the sealing ring.

8. The 3D microemulsion preparation device according to claim 1, It is characterized in that The material of the generating nozzle and the material of the collecting device are both compatible with 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 spacing between the generating nozzle and the collecting device ranges from 10 μm to 500 μm.

9. A method for preparing microemulsion droplets, It is characterized in that The 3D microemulsion preparation device according to any one of claims 1 to 8 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: The capillary tube through which the continuous phase passes is fixedly connected to the delivery pipeline on the feeding side, one end of the collecting capillary tube is fixedly connected to the delivery pipeline on the collecting side, and the other end of the collecting capillary tube is connected to the collecting container; S3: placing the preparation body vertically so that the top exhaust pipe is above the preparation cavity, passing the continuous phase into the preparation cavity at a target flow rate, and observing the filling process of the continuous phase in the preparation cavity through a transparent window. When the preparation cavity is full of the continuous phase, plugging the top exhaust pipe with a plug and reducing the flow rate of the continuous phase; S4: removing the plug installed on the generation side delivery pipeline, fixing the capillary tube through which the dispersed phase passes to the generation side delivery pipeline, introducing the dispersed phase into the preparation cavity at a target flow rate, generating microemulsion droplets of target size and target frequency distribution in the preparation cavity, and delivering the generated microemulsion droplets into the collection container through the collection tube in the preparation cavity.

10. The method for preparing microemulsion droplets according to claim 9, It is characterized in that In step S3, if bubbles are generated during the filling process of the continuous phase, the preparation body is gently shaken so that the air in the preparation body is 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 introduced into the preparation cavity and / or the flow rate of the continuous phase introduced into the preparation cavity.

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