A temperature-controlled double-emulsion droplet batch preparation system and method

By changing the surface tension of the emulsion within the sandwich cavity of the chip processing unit using a temperature control device, the batch preparation of dual emulsion droplets was achieved, solving the problems of low preparation efficiency and high cost in existing technologies, and realizing efficient and low-cost dual emulsion droplet processing.

CN115779752BActive Publication Date: 2026-01-13SHAANXI UNIV OF CHINESE MEDICINE +1
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Patent Information

Application Number
CN202211242942.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-10-11
Publication Date
2026-01-13
Estimated Expiration
2042-10-11

AI Technical Summary

Technical Problem

Existing technologies for preparing dual emulsion droplets are inefficient and costly, and the stringent reliability requirements of microfluidic chips further increase processing costs.

Method used

A temperature-controlled dual-emulsion droplet batch preparation system is adopted. By using a temperature control device to heat or cool the emulsion in the sandwich cavity of the chip, the surface tension of the dispersed liquid is changed, forming an injection mechanical force to inject the continuous liquid into the droplets to form sub-droplets, thus realizing the batch preparation of dual-emulsion droplets.

Benefits of technology

It greatly improves the preparation efficiency of dual emulsion droplets, reduces processing costs, and avoids limitations on material properties through non-contact processing, making it suitable for batch processing of dual emulsion droplets with different material compositions.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a kind of based on temperature control's double emulsion drop batch preparation system, comprising: processing chip, temperature control device, injector and droplet collector;Processing chip is provided with interlayer cavity;Processing chip is contacted with temperature control device;Temperature control device is used to heat or cool the whole emulsion to be processed in interlayer cavity, to make the whole dispersed phase liquid of emulsion to be processed in interlayer cavity simultaneously form double emulsion drop;Processing chip is provided with and interlayer cavity two ends communication liquid inlet and liquid outlet;Liquid inlet is communicated with the outlet of injector, and outlet is communicated with droplet collector.The application also provides a kind of based on temperature control's double emulsion drop batch preparation method.The application can realize the purpose of batch assembly double emulsion drop, greatly improves the preparation efficiency of double emulsion.Meanwhile, using temperature control device controls the ambient temperature of emulsion to be processed, simple structure, reduces processing cost.
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Description

Technical Field

[0001] This invention belongs to the field of dual emulsion droplet preparation technology, specifically relating to a temperature-controlled dual emulsion droplet batch preparation system and preparation method. Background Technology

[0002] An emulsion is a mixture of two or more immiscible liquids, in which one liquid (dispersed phase) is distributed as droplets within another liquid (continuous phase). Further, a biemulsion (also known as a dual emulsion) is an emulsion within an emulsion or encapsulated droplets, i.e., a highly structured fluid in which smaller droplets (sub-droplets) are encapsulated within droplets of a dispersed liquid. Typical types are water-in-oil-in-water (W / O / W) and oil-in-water-in-oil (O / W / O) types. The characteristic size of biemulsion droplets is typically in the range of hundreds of nanometers to millimeters (mesoscopic scale), offering significant advantages such as low reagent consumption, minimal cross-contamination, and ease of manipulation. Furthermore, as a closed microsphere, the sub-droplets within it can load and store various entrained substances, such as bioactive substances or active ingredients requiring environmental chemical protection (oxidation, decomposition, hydrolysis), making it widely applicable in various fields including medicine and life sciences, biopharmaceuticals, food engineering, cosmetic engineering, and chemical engineering.

[0003] Currently, the fabrication of biemulsion droplets commonly employs droplet microfluidics. This technology utilizes microfluidic chips with different structures to control the convection of immiscible liquids, forming microdroplets under shearing and extrusion. Microdroplet spherical structures are then assembled in two or more steps, achieving preliminary controllable design and manipulation of the size, morphology, and function of biemulsion droplets. However, based on the processing principle of droplet microfluidics, biemulsion droplets are generated one by one. Even with various methods such as increasing flow rates and optimizing microchannel design, the droplet preparation efficiency remains low. Furthermore, high-speed fluid flow places stringent reliability requirements on microfluidic chips, while microfluidic chips with complex microchannel designs are expensive, further increasing the cost of biemulsion droplet fabrication. Summary of the Invention

[0004] To address the aforementioned problems in the prior art, this invention provides a temperature-controlled batch preparation system and method for dual emulsion droplets.

[0005] A first aspect of the present invention provides a temperature-controlled dual emulsion droplet batch preparation system, comprising: a processing chip, a temperature control device, a syringe, and a droplet collector;

[0006] The processed chip has a sandwich cavity inside;

[0007] The processed chip is in contact with the temperature control device;

[0008] The temperature control device is used to heat or cool all the emulsion to be processed in the sandwich cavity so that all the liquid droplets of the dispersed phase of the emulsion to be processed in the sandwich cavity simultaneously form double emulsion droplets.

[0009] The processing chip is provided with an inlet and an outlet that are connected to both ends of the interlayer cavity;

[0010] The inlet is connected to the outlet of the syringe, and the outlet is connected to the droplet collector.

[0011] In one embodiment of the present invention, the processed chip includes: an upper substrate and a lower substrate; the temperature control device includes: an upper heat exchange device and a lower heat exchange device;

[0012] The sandwich cavity is formed between the upper substrate and the lower substrate;

[0013] The upper heat exchange device is attached to and covers the outer surface of the upper substrate;

[0014] The lower heat exchange device is attached to and covers the outer surface of the lower substrate.

[0015] In one embodiment of the present invention, a circulating water bath device is also included;

[0016] Both the upper heat exchange device and the lower heat exchange device are liquid storage devices;

[0017] The circulating water bath device is connected to the upper heat exchange device and the lower heat exchange device.

[0018] In one embodiment of the present invention, the inlet is connected to the outlet of the syringe via an inlet pipe;

[0019] The liquid outlet is connected to the droplet collector via a liquid outlet pipe.

[0020] In one embodiment of the present invention, a first micro fluid solenoid valve is installed on the inlet pipe near the inlet port;

[0021] A second micro fluid solenoid valve is installed near the outlet of the liquid outlet pipe.

[0022] In one embodiment of the present invention, two microfluidic peristaltic injection pumps are also included;

[0023] One of the microfluidic peristaltic injection pumps is connected to the syringe, and the other microfluidic peristaltic injection pump is connected to the outlet.

[0024] A second aspect of this invention provides a temperature-controlled method for batch preparation of dual emulsion droplets, applied to a temperature-controlled dual emulsion droplet batch preparation system described in the first aspect of this invention, comprising the following steps:

[0025] Step 1: Install and connect the processed chip, temperature control device, syringe, and droplet collector;

[0026] Step 2: Control the syringe to inject the emulsion to be processed into the interlayer cavity through the inlet of the processed chip; the emulsion to be processed includes a dispersed phase liquid and a continuous phase liquid;

[0027] Step 3: Control the temperature of the temperature control device to increase or decrease, so that all the emulsions to be processed in the interlayer cavity are heated or cooled within a preset time, so as to achieve the simultaneous formation of double emulsion droplets from all the dispersed liquid phases of the emulsions to be processed in the interlayer cavity.

[0028] Step four: Discharge the dual emulsion droplets from the interlayer cavity into the droplet collector.

[0029] In one embodiment of the present invention, step three specifically includes the following steps:

[0030] Step 31: Control the temperature of the temperature control device to increase or decrease, so that all the emulsion to be processed in the interlayer cavity is heated to the first preset temperature or cooled to the second preset temperature within a first preset time.

[0031] Step 32: Control the temperature of the temperature control device to decrease or increase, so that all the emulsion to be processed in the interlayer cavity is cooled to a third preset temperature or heated to a fourth preset temperature within a second preset time.

[0032] Step 33: Repeat steps 31 and 32 in sequence multiple times.

[0033] In particular, steps 31, 32 and 33 can all enable the simultaneous formation of double emulsion droplets from all the dispersed phase liquids of the emulsion to be processed within the sandwich cavity.

[0034] The beneficial effects of this invention are:

[0035] This invention controls the temperature of the processed chip using a temperature control device, thereby raising or lowering the temperature of all the emulsion to be processed within the sandwich cavity. By controlling the ambient temperature of the emulsion, the surface tension of the dispersed phase liquid droplets in the emulsion is altered, thus creating an injection mechanical force at the droplet's spherical interface. This injects the continuous phase liquid of the emulsion into the droplet, forming sub-droplets within it. Consequently, all the dispersed phase liquid droplets simultaneously form biemulsion droplets, achieving the goal of batch assembly of biemulsion droplets and significantly improving the preparation efficiency of biemulsions. Furthermore, the use of a temperature control device to control the ambient temperature of the emulsion is simple in structure, technologically mature, and reduces processing costs.

[0036] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0037] Figure 1 A schematic diagram of the installation structure of a fabricated chip and a temperature control device for a temperature-controlled dual-emulsion droplet batch preparation system provided in this embodiment of the invention:

[0038] Figure 2 A schematic diagram of the processing chip and temperature control device for injecting emulsion into an embodiment of the present invention;

[0039] Figure 3 A top view of the processed chip provided in an embodiment of the present invention;

[0040] Figure 4 A schematic diagram of a temperature-controlled dual emulsion droplet batch preparation system provided in an embodiment of the present invention;

[0041] Figure 5 The images show the microstructure of the emulsion to be processed and the dual emulsion, as well as the structural schematic diagrams of the corresponding droplets and dual emulsion droplets, used in the batch preparation of dual emulsion droplets according to Embodiment 3 of the present invention.

[0042] Figure 6 These are microscopic texture images of the double emulsion droplets after one, two, and three temperature injection cycles according to Embodiment 4 of the present invention.

[0043] Figure 7 This is a microscopic texture image of a double emulsion droplet after multiple temperature injection cycles in Embodiment 4 of the present invention.

[0044] Figure 8 This is a schematic diagram illustrating the relationship between interfacial tension and temperature, provided in an embodiment of the present invention.

[0045] Figure 9 This is a schematic diagram illustrating the relationship between the number of injected sub-droplets and the volume of the dual emulsion droplets and the number of injections in Embodiment 4 of the present invention.

[0046] Figure 10This is a schematic diagram of the size distribution of the injected droplets in Embodiment 4 of the present invention;

[0047] Figure 11 This is a schematic diagram of the volume distribution of the double emulsion droplets in Embodiment 4 of the present invention.

[0048] Explanation of reference numerals in the attached figures:

[0049] 10-Processed chip; 11-Interlayer cavity; 12-Upper substrate; 13-Lower substrate; 14-Droplet to be processed; 15-Continuous phase liquid; 21-Upper heat exchange device; 22-Lower heat exchange device; 30-Injector; 31-Emulsion to be processed; 40-Droplet collector; 50-Inlet pipe; 51-First microfluidic solenoid valve; 60-Outlet pipe; 61-Second microfluidic solenoid valve; 70-Dual emulsion droplet; 71-Sub-droplet. Detailed Implementation

[0050] The present invention will be further described in detail below with reference to specific embodiments, but the implementation of the present invention is not limited thereto.

[0051] Example 1

[0052] like Figure 1 , Figure 2 , Figure 3 , Figure 4 and Figure 5 As shown, a first aspect of the present invention provides a temperature-controlled dual emulsion droplet batch preparation system, comprising: a processing chip 10, a temperature control device, a syringe 30, and a droplet collector 40. The processing chip 10 has a sandwich cavity 11. The processing chip 10 is in contact with the temperature control device.

[0053] The temperature control device is used to heat or cool all the emulsion to be processed in the sandwich cavity 11, so that all the dispersed phase liquid droplets 14 of the emulsion to be processed in the sandwich cavity 11 simultaneously form double emulsion droplets 70. The temperature control device can regulate and control the temperature of the processing chip 10, thereby regulating the ambient temperature of the emulsion to be processed in the sandwich cavity 11 of the processing chip 10. By controlling the change of the ambient temperature of the emulsion, the surface tension (i.e., interfacial tension) of the dispersed phase liquid droplets 14 in the emulsion to be processed is changed, thereby forming an injection mechanical force at the spherical interface of the droplets 14 to be processed, injecting the continuous phase liquid 15 of the emulsion to be processed into the droplets 14, forming sub-droplets 71 in the droplets, thus realizing the simultaneous assembly of all the dispersed phase liquid droplets 14 to be processed into double emulsion droplets 70, achieving the purpose of batch preparation of double emulsions.

[0054] The processed chip 10 is provided with an inlet and an outlet that are connected to both ends of the interlayer cavity 11. The inlet is connected to the outlet of the syringe 30, and the outlet is connected to the droplet collector 40.

[0055] In this embodiment, the emulsion 31 to be processed is injected into the interlayer cavity 11 of the processing chip 10 through the syringe 30. Then, the processing chip 10 is heated or cooled by the temperature control device, so that the temperature of the emulsion to be processed in the interlayer cavity 11 is raised or lowered, and the emulsion to be processed forms a double emulsion. The double emulsion droplets 70 enter the droplet collector 40 through the liquid outlet, so as to collect the processed double emulsion droplets 70.

[0056] In this embodiment, the temperature of the processed chip 10 is controlled by a temperature control device, thereby raising or lowering the temperature of all the emulsion to be processed in the interlayer cavity 11. By controlling the ambient temperature of the emulsion to be processed, the surface tension of all the droplets 14 of the dispersed phase liquid in the emulsion is changed, thereby forming an injection mechanical force at the spherical interface of all the droplets 14 to be processed, injecting the continuous phase liquid of the emulsion to be processed into the droplets 14 to be processed, forming sub-droplets 71 within the droplets. Thus, all the droplets 14 of the dispersed phase liquid simultaneously form double emulsion droplets 70, achieving the purpose of batch assembly of double emulsion droplets 70. At the same time, the use of a temperature control device to control the ambient temperature of the emulsion to be processed is simple in structure, greatly improving the preparation efficiency of double emulsions while reducing processing costs. It has important scientific and technological value for promoting the technological progress and large-scale application of extreme manufacturing of double emulsion droplets.

[0057] The dual-emulsion droplet batch preparation system of this embodiment realizes batch, precision micro-nano processing of dual-emulsion droplets, which is more efficient than the traditional method of processing droplets one by one. The dual-emulsion droplet batch preparation system performs precision processing in a non-contact manner by controlling temperature variables, which eliminates the limitations of material properties such as material flowability, shear resistance, and diffusion in traditional contact processing technology. It can be widely applied to the batch processing of water-in-oil-in-water (W / O / W) and oil-in-water-in-oil (O / W / O) dual-emulsion droplets with different material compositions.

[0058] It should be noted that changes in the temperature of the emulsion can cause changes in interfacial tension, leading to convection in the fluid material and making the interface unstable. This creates injection mechanical forces at the interface, allowing the continuous liquid phase to be injected into the droplets. Rapid temperature increases or decreases can cause rapid changes in interfacial tension, resulting in significant injection mechanical forces. By controlling the rapid rise or fall of the emulsion's ambient temperature, a sudden temperature change is created, generating significant injection mechanical forces on the surface of all droplets in the emulsion to be processed. This injects the solution into the droplets, forming sub-droplets within them, thus achieving large-scale, batch processing (high-efficiency) of dual emulsion droplets in a non-contact manner.

[0059] In one embodiment, the chip processing 10 includes an upper substrate 12 and a lower substrate 13; the temperature control device includes an upper heat exchange device 21 and a lower heat exchange device 22.

[0060] A sandwich cavity 11 is formed between the upper substrate 12 and the lower substrate 13. The upper heat exchange device 21 is attached to the outer surface of the upper substrate 12 and covers the outer surface of the upper substrate 12. The lower heat exchange device 22 is attached to the outer surface of the lower substrate 13 and covers the outer surface of the lower substrate 13.

[0061] In this embodiment, when the upper heat exchanger 21 and the lower heat exchanger 22 are working, they can change the temperature inside the sandwich cavity 11, raising or lowering the temperature of the emulsion to be processed. The effective working area of ​​the upper heat exchanger 21 and the lower heat exchanger 22 completely covers the upper substrate 12 and the lower substrate 13.

[0062] For example, depending on different processing requirements, the upper heat exchanger 21 and the lower heat exchanger 22 can be equipped with temperature control devices such as glass / metal heat carriers and semiconductor heaters (such as Peltier patches), or heat exchanger devices that have both heating and cooling functions can be used. Preferably, a typical model is the Jingtong glass heat carrier HS72.

[0063] In one embodiment, the chip 10 is made of glass, or it may be made of other materials with good thermal conductivity, such as metal.

[0064] In one embodiment, the temperature control device further includes a circulating water bath. Both the upper heat exchanger 21 and the lower heat exchanger 22 are liquid storage devices, connected to the circulating water bath. Solutions of different temperatures are introduced into the upper and lower heat exchangers 21 and 22 through the circulating water bath, enabling rapid temperature increases and decreases in the upper and lower heat exchangers 21 and 22. This controls the temperature of the processed chip 10, thereby raising or lowering the temperature of all the emulsion to be processed within the interlayer cavity 11. Water bath temperature control allows for rapid temperature increases and decreases (rapidly replacing solutions of different temperatures within the liquid storage devices achieves rapid temperature changes), thus improving processing efficiency. The upper and lower heat exchangers 21 and 22 are made of materials with good thermal conductivity.

[0065] Furthermore, the inlet is connected to the outlet of the syringe 30 via the inlet tube 50. The outlet is connected to the droplet collector 40 via the outlet tube 60.

[0066] In one feasible implementation, the inner diameter of both the inlet pipe 50 and the outlet pipe 60 is 0.1mm-4mm.

[0067] Furthermore, a first microfluidic solenoid valve 51 is installed near the inlet of the inlet pipe 50. A second microfluidic solenoid valve 61 is installed near the outlet of the outlet pipe 60. These microfluidic solenoid valves are used to block the diffusion of temperature and substances between the processed chip 10 and the emulsion in the inlet and outlet pipes 50 during processing.

[0068] Furthermore, it also includes two microfluidic peristaltic injection pumps. One microfluidic peristaltic injection pump is connected to the syringe 30 and is used to deliver the emulsion 31 to be processed in the syringe 30 into the interlayer cavity 11 of the processing chip 10. The other microfluidic peristaltic injection pump is connected to the outlet and is used to discharge the processed dual emulsion from the interlayer cavity 11 of the processing chip 10.

[0069] In one feasible implementation, the microfluidic peristaltic injection pump is a Harvard pump33. The droplet collector 40 is a Xiangbo glass sample vial XB-YPP.

[0070] Example 2

[0071] like Figure 1 , Figure 2 , Figure 3 and Figure 4 As shown, a second aspect of the present invention provides a method for batch preparation of dual emulsion droplets based on temperature control, applicable to the batch preparation of dual emulsion droplets using the preparation system in Example 1, comprising the following steps:

[0072] Step 1: Install and connect the processing chip 10, temperature control device, syringe 30 and droplet collector 40; the processing chip 10 is in contact with the temperature control device; the liquid inlet is connected to the outlet of the syringe 30, and the liquid outlet is connected to the droplet collector 40.

[0073] Step two: Control the syringe 30 to inject the emulsion 31 to be processed into the jacketed cavity 11 through the inlet of the processing chip 10; the emulsion to be processed includes a dispersed liquid phase and a continuous liquid phase; the jacketed cavity 11 can be injected with the emulsion to be processed and maintain good airtightness. The thickness of the jacketed cavity 11 (typically 0.3-5 mm) should be greater than the diameter of the droplets 14 to be processed in the emulsion to be processed (typically 0.01-5 mm).

[0074] Step 3: The temperature of the temperature control device is raised or lowered to raise or lower the temperature of all the emulsions to be processed in the interlayer cavity 11 within a preset time. This achieves the simultaneous formation of double emulsion droplets 70 from all the dispersed phase liquid droplets 14 of the emulsions to be processed within the interlayer cavity 11. The temperature control device controls the temperature of the processing chip 10, thereby rapidly raising or lowering the temperature of all the emulsions to be processed within the interlayer cavity 11 within a preset time. By controlling the ambient temperature of the emulsions to be processed, the surface tension of all the dispersed phase liquid droplets 14 in the emulsion is changed. This creates an injection mechanical force at the spherical interface of all the droplets 14, injecting the continuous phase liquid of the emulsion into the droplets 14 to form sub-droplets 71 within the droplets. Thus, all the dispersed phase liquid droplets 14 simultaneously form double emulsion droplets 70, achieving the purpose of batch assembly of double emulsion droplets. At the same time, the use of a temperature control device to control the ambient temperature of the emulsions to be processed is simple in structure and greatly improves the preparation efficiency of double emulsions while reducing processing costs.

[0075] Step four: Discharge the double emulsion droplets 70 from the interlayer cavity 11 into the droplet collector 40.

[0076] In one feasible implementation, step three includes steps 31-33.

[0077] Step 31: Control the temperature of the temperature control device to increase or decrease, so that all the emulsion to be processed in the interlayer cavity 11 is heated to the first preset temperature or cooled to the second preset temperature within a first preset time.

[0078] Step 32: Control the temperature of the temperature control device to decrease or increase, so that all the emulsion to be processed in the interlayer cavity 11 is cooled to the third preset temperature or heated to the fourth preset temperature within a second preset time.

[0079] Step 33: Repeat steps 31 and 32 in sequence multiple times; Steps 31 to 32 constitute one temperature injection cycle, and this temperature injection cycle is repeated multiple times.

[0080] In particular, steps 31, 32 and 33 can all achieve the simultaneous formation of double emulsion droplets 70 from all the dispersed phase liquid droplets 14 of the emulsion to be processed in the interlayer cavity 11.

[0081] For example, in processing a biemulsion, a heating process is first performed to rapidly change the temperature of the emulsion within a first preset time period, causing all the dispersed liquid droplets 14 of the emulsion to be processed within the sandwich cavity 11 to simultaneously form biemulsion droplets 70. Then, a cooling process is performed to rapidly change the temperature of the emulsion again within a second preset time period, continuing to form biemulsion droplet structures. This heating and cooling cycle constitutes one temperature injection cycle, and repeating this temperature injection cycle at least once can produce the final biemulsion droplets.

[0082] Accordingly, when processing dual emulsions, a cooling process can be performed first, followed by a heating process, as a temperature injection cycle.

[0083] During a temperature injection cycle, a certain volume of continuous phase liquid 15 is injected into the droplet 14 to be processed to form a double emulsion droplet. As the temperature injection cycle is repeated multiple times, the number of injected sub-droplets 71 will continue to increase. Eventually, the double emulsion droplet is filled with injected sub-droplets 71 and all the double emulsion droplets have a high degree of structural homogeneity.

[0084] Example 3

[0085] like Figure 5 As shown, a temperature-controlled method for batch preparation of dual emulsion droplets is applied to the batch preparation of dual emulsion droplets using the preparation system in Example 1, and includes the following steps:

[0086] Step S31: Install and connect the processing chip 10, temperature control device, syringe 30, and droplet collector 40; the processing chip 10 is in contact with the temperature control device; the liquid inlet is connected to the outlet of the syringe 30, and the liquid outlet is connected to the droplet collector 40. The upper heat exchange device 21 and lower heat exchange device 22 of the temperature control device are Jingtong glass heat carrier stages HS72.

[0087] In step S32, the syringe 30 is controlled to inject the emulsion 31 to be processed into the interlayer cavity 11 through the liquid inlet of the processing chip 10; the emulsion to be processed includes a dispersed phase liquid and a continuous phase liquid; the interlayer cavity 11 can be injected with the emulsion to be processed and maintain good airtightness.

[0088] The emulsion materials used are liquid crystal E7 (Merck) and deionized water. The aqueous solution is doped with 0.5 wt% of surfactant SDS (sodium lauryl sulfate, Sigma-Aldrich) to enable the droplets to be processed to be stably suspended in water to form an emulsion.

[0089] Step S33: The temperature of the temperature control device is increased to rapidly raise the temperature of all the emulsion to be processed in the interlayer cavity 11 to 50°C within a preset time of 30 seconds, so as to simultaneously form double emulsion droplets 70 from all the dispersed liquid droplets 14 of the emulsion to be processed in the interlayer cavity 11. Specifically, due to the temperature change in the interlayer cavity 11, an injection mechanical force is generated in the emulsion to be processed, injecting the aqueous solution into the droplets 14 to form uniformly sized sub-droplets 71. The injected sub-droplets 71 spontaneously organize and align into a droplet chain structure according to the molecular orientation field within the droplet (the liquid crystal molecules in the droplet are arranged radially like spheres), forming double emulsion droplets 70, as shown below. Figure 5 As shown.

[0090] Step S34: The double emulsion droplets 70 are discharged from the interlayer cavity 11 into the droplet collector 40.

[0091] In one feasible implementation, in step S33, the temperature of the temperature control device can also be controlled to decrease so that all the emulsion to be processed in the interlayer cavity 11 can be rapidly cooled from room temperature to 5°C within a preset time of 30 seconds.

[0092] Example 4

[0093] A method for batch preparation of dual emulsion droplets based on temperature control includes the following steps:

[0094] Step S41: Install and connect the processing chip 10, temperature control device, syringe 30 and droplet collector 40; the processing chip 10 is a glass chip; the temperature control device is a circulating water bath device, and an upper heat exchange device 21 and a lower heat exchange device 22 connected to it; the liquid inlet is connected to the outlet of the syringe 30, and the liquid outlet is connected to the droplet collector 40.

[0095] In step S42, the syringe 30 is controlled to inject the emulsion 31 to be processed into the interlayer cavity 11 through the liquid inlet of the processing chip 10; the emulsion to be processed includes a dispersed phase liquid and a continuous phase liquid; the interlayer cavity 11 can be injected with the emulsion to be processed and maintain good airtightness.

[0096] The emulsion uses liquid crystal E7 (Merck) and deionized water, and the aqueous solution is doped with 0.5 wt% of surfactant SDS (sodium lauryl sulfate, Sigma-Aldrich).

[0097] Step S43: Control the temperature of the circulating water bath device to keep the temperature of the upper heat exchanger 21 and the lower heat exchanger 22 at 50°C, so that all the emulsion to be processed in the jacket cavity 11 can be heated from room temperature to 50°C within 30 seconds.

[0098] Step S44: Within 4 seconds, 10 ml of cool water at 25°C is quickly added to the circulating water bath device to cause a brief and rapid drop in temperature in the upper heat exchange device 21 and the lower heat exchange device 22, so as to rapidly reduce the temperature of all the emulsions to be processed.

[0099] Step S45: Repeat steps S43 to S44 multiple times. Steps S43-S44 constitute one temperature injection cycle, which is repeated several times. The droplet structures of the biemulsion after one, two, and three temperature injection cycles are as follows: Figure 6 and Figure 7 As shown in the image.

[0100] It should be noted that, as Figure 8 As shown, the relationship between the temperature and interfacial tension of the emulsion exhibits a linear change. Convection occurs in the fluid material, making the interface unstable and thus generating injection mechanical force, allowing the continuous liquid phase to be injected into the droplet. Rapid temperature rises and falls can cause rapid changes in interfacial tension, thereby generating a large injection mechanical force.

[0101] like Figure 9 As shown, Figure 9 for Figure 6 Measurement data from multiple injections showed a good linear relationship between the number of injected sub-droplets (bar chart) and the volume of the biemulsion droplets (line chart) and the number of injections (temperature injection cycle). This indicates that the number of sub-droplets injected in each temperature change cycle is similar, and the volume of the aqueous solution (continuous phase) injected in each cycle is similar.

[0102] At the same time, such as Figure 10 and Figure 11 As shown, Figure 10 for Figure 7 The bar chart shows the size distribution of sub-droplets injected into the double emulsion droplet (the curve in the figure is a fitted Gaussian curve), indicating that the sub-droplet size uniformity is good. Figure 11 for Figure 7 The histogram of the volume distribution of the dual emulsion droplets in this embodiment (the curve is a fitted Gaussian curve) shows that the dual emulsion droplets processed by the method in this embodiment have good size uniformity (close to the dual emulsion droplets generated by traditional microfluidic technology).

[0103] Therefore, the resulting biemulsion droplet structure has a high degree of homogeneity.

[0104] In one feasible implementation, a large-sized dual-emulsion droplet processing chip 10 is selected. Preferably, the size of the processing chip 10 is 300mm*300mm.

[0105] It should be noted that the efficiency of processing dual emulsion droplets using traditional microfluidic technology (processing one droplet at a time) is approximately on the order of 0.7 mL / hr. Taking a 300*300 mm chip as an example, the efficiency of processing dual emulsion droplets using the temperature control method of Embodiment 4 of this invention is on the order of approximately 54 mL / hr.

[0106] It should be noted that although only water baths, heated stages and other temperature control methods are listed in this invention, the injection of materials at the interface of immiscible fluids using other temperature control methods to achieve the micro-nano fabrication of double emulsion droplets is within the scope of protection of this invention.

[0107] Although this invention only lists emulsion systems composed of materials such as liquid crystal and water, any technical method for processing double emulsion droplets by simply replacing different material components and mechanically injecting them at the fluid-material interface using temperature is within the scope of protection of this invention.

[0108] Although this invention only demonstrates the batch processing of double emulsion droplets within the 10-cavity size of a cuboid-shaped chip, any technical solution that uses temperature control to inject a solution into droplets of any size, shape, and quantity to form double emulsion droplets is within the scope of protection of this invention.

[0109] This invention utilizes temperature manipulation to alter the surface tension of droplets within an emulsion, generating mechanical force for the precision machining of dual emulsion droplets. Employing a mature and cost-effective temperature control scheme, all emulsion droplets within the processing chip 10 can be processed simultaneously, significantly reducing the cost of dual emulsion droplet machining while achieving extremely high processing efficiency and precision. The non-contact machining method has low requirements for material physical properties, making it widely applicable to the extreme machining of dual emulsion droplets.

[0110] In this invention, the number and size of the injected sub-droplets, i.e. the volume of the injected solution, can be precisely controlled by controlling the number of temperature changes, thereby achieving high-precision micro-nano fabrication.

[0111] In this invention, all droplets within the processing chip 10 can be micro-nano-processed simultaneously within the same temperature cycle, resulting in extremely high processing efficiency.

[0112] The preparation method of the present invention is applicable to the large-scale precision processing of double emulsion droplets of arbitrary shape, size, scale, and composition, providing a reliable extreme processing technology for exploring new applications and developing large-scale applications.

[0113] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," and "counterclockwise," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0114] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.

[0115] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0116] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0117] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. In addition, those skilled in the art can combine and integrate the different embodiments or examples described in this specification.

[0118] The above description, in conjunction with specific preferred embodiments, provides a further detailed explanation of the present invention. It should not be construed that the specific implementation of the present invention is limited to these descriptions. For those skilled in the art, various simple deductions or substitutions can be made without departing from the concept of the present invention, and all such modifications and substitutions should be considered within the scope of protection of the present invention.

Claims

1. A temperature control based double emulsion droplet batch production system, characterized in that, The application relates to a temperature-controlled double emulsion droplet batch preparation system. The system comprises a processing chip (10), a temperature control device, an injector (30) and a droplet collector (40). The processing chip (10) is provided with a sandwich cavity (11). The processing chip (10) is in contact with the temperature control device. The temperature control device is used for heating or cooling all emulsions to be processed in the sandwich cavity (11) so that all dispersed phase liquid droplets (14) in the emulsions to be processed in the sandwich cavity (11) are simultaneously formed into double emulsion droplets (70); wherein the temperature control device changes the surface tension distribution of the dispersed phase liquid droplets (14) in the emulsions to be processed by controlling the emulsion environment temperature change, so that an injection mechanical force is formed at the spherical interface of the dispersed phase liquid droplets (14) to inject the continuous phase liquid (15) of the emulsions to be processed into the dispersed phase liquid droplets (14) and form sub-droplets (71) in the droplets, thereby realizing the simultaneous assembly of all dispersed phase liquid droplets (14) into double emulsion droplets (70). The processing chip (10) is provided with an inlet and an outlet which are in communication with both ends of the sandwich cavity (11); the processing chip (10) comprises an upper substrate (12) and a lower substrate (13); the temperature control device comprises an upper heat exchange device (21) and a lower heat exchange device (22). The sandwich cavity (11) is formed between the upper substrate (12) and the lower substrate (13). The upper heat exchange device (21) is in contact with and covers the outer surface of the upper substrate (12). The lower heat exchange device (22) is in contact with and covers the outer surface of the lower substrate (13). The inlet is in communication with the outlet of the injector (30), and the outlet is in communication with the droplet collector (40).

2. A temperature-controlled based double emulsion droplet batch production system according to claim 1, wherein, The temperature control device further comprises a circulating water bath device. The upper heat exchange device (21) and the lower heat exchange device (22) are both liquid storage devices. The circulating water bath device is in communication with the upper heat exchange device (21) and the lower heat exchange device (22).

3. A temperature-controlled based double emulsion droplet batch production system according to claim 1, wherein, The inlet is in communication with the outlet of the injector (30) through an inlet pipe (50). The outlet is in communication with the droplet collector (40) through an outlet pipe (60).

4. A double emulsion droplet batch production system based on temperature control according to claim 3, characterized in that, A first micro fluid electromagnetic valve (51) is installed at a position close to the inlet of the inlet pipe (50). A second micro fluid electromagnetic valve (61) is installed at a position close to the outlet of the outlet pipe (60).

5. A temperature-controlled based double emulsion droplet batch production system according to claim 3, wherein, Two micro fluid peristaltic injection pumps are further included. One of the micro fluid peristaltic injection pumps is in communication with the injector (30), and the other is in communication with the outlet.

6. A method for batch production of double emulsion droplets based on temperature control, characterized in that, The application is applied to the temperature-controlled double emulsion droplet batch preparation system as claimed in any one of claims 1-5 and comprises the following steps. Step one, install and connect the processing chip (10), the temperature control device, the injector (30) and the droplet collector (40). Step two, control the syringe (30) to inject the emulsion to be processed (31) into the sandwich cavity (11) through the inlet of the processing chip (10); the emulsion to be processed (31) includes dispersed phase liquid and continuous phase liquid; Step three, control the temperature control device to increase or decrease the temperature, so that all the emulsion to be processed in the sandwich cavity (11) is heated or cooled within a preset time, so that all the droplets to be processed (14) of the dispersed phase liquid in the emulsion to be processed in the sandwich cavity (11) form double emulsion droplets (70) at the same time; wherein, the temperature control device changes the surface tension distribution of the droplets to be processed (14) of the dispersed phase liquid in the emulsion to be processed by controlling the change of the emulsion environment temperature, so as to form an injection mechanical force at the spherical interface of the droplets to be processed (14) to inject the continuous phase liquid (15) of the emulsion to be processed into the droplets to be processed (14), form sub-droplets (71) in the droplets, and realize the simultaneous assembly of all the droplets to be processed (14) of the dispersed phase liquid to form double emulsion droplets (70); Step four, discharge the double emulsion droplets (70) from the sandwich cavity (11) to the droplet collector (40).

7. A method of batch production of double emulsion droplets based on temperature control according to claim 6, characterized in that, The specific steps of step three include: Step 31, control the temperature control device to increase or decrease the temperature, so that all the emulsion to be processed in the sandwich cavity (11) is heated to a first preset temperature or cooled to a second preset temperature within a first preset time; Step 32, control the temperature control device to increase or decrease the temperature, so that all the emulsion to be processed in the sandwich cavity (11) is cooled to a third preset temperature or heated to a fourth preset temperature within a second preset time; Step 33, repeatedly perform the step 31 and the step 32 in sequence for multiple times; Wherein, steps 31, 32 and 33 can all realize the formation of double emulsion droplets (70) by all the droplets to be processed (14) of the dispersed phase liquid in the emulsion to be processed in the sandwich cavity (11).

Citation Information

Patent Citations

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    CN114225977A