Micro-droplet generating and collecting device

By designing a micro droplet generation and collection device, using a -80°C refrigeration system and a snake-shaped condensing tube to achieve efficient collection of micro droplets, solving the problem of difficult collection of micro droplets in the prior art and improving the micro droplet reaction Efficiency and application value.

CN119319005APending Publication Date: 2025-01-17TIANJIN MICRODROPLET INNOVATION TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411468431.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-21
Publication Date
2025-01-17

AI Technical Summary

Technical Problem

The prior art is difficult to achieve efficient collection of high-speed flying microdroplets, resulting in inefficiency in chemical reactions of microdroplets and small-scale synthesis.

Method used

A micro droplet generation and collection device is designed, including a -80°C refrigeration system, a micro droplet preparation system and a collection system, which generates micro droplets through carrier gas devices, tee fittings and syringe pumps, and uses a snake-shaped condenser tube. Achieve frozen collection to ensure efficient preparation and collection of micro droplets.

Benefits of technology

It realizes efficient collection of micro droplets, simplifies operation, improves the efficiency of micro droplet reaction, does not affect the reaction rate, and has high application value.

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Abstract

The invention discloses a device for generating and collecting micro-droplets. The device comprises a-80 DEG C refrigerating system, a micro-droplet preparation system and a collecting system. Wherein a liquid outlet pipe and a liquid inlet pipe of the-80 DEG C refrigerating system are respectively inserted into a condensate inlet and a condensate outlet of the collecting system; the micro-droplet preparation system consists of a carrier gas device, a three-way pipe fitting and an injection pump; liquid drops of liquid injected by the injection pump are scattered into micro liquid drops by high-pressure carrier gas; the collecting system is a glass device similar to a U shape and is communicated with the micro-droplet blowing-in end on the left side, the liquid taking opening in the bottom and the gas outlet on the right side; the micro-droplet reaction is completed at the micro-droplet blowing-in end, and the micro-droplets are condensed in the S-shaped condensation pipe of the U-shaped glass device and then are collected through a liquid taking opening in the bottom. According to the device, a micro-droplet generating device and a micro-droplet collecting device are ingeniously integrated into one device, so that the device is simple in structure and convenient to operate, ultra-high-efficiency micro-droplet collection can be achieved, and the device has very high application value.
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Description

Technical Field

[0001] The present invention relates to the field of micro-droplet chemistry, and in particular to the technology of micro-droplet preparation and efficient collection Background Art

[0002] Water has long been considered a stable and relatively inert liquid, and therefore can serve as a solvent for many chemical reaction systems. In recent years, scientific research has found that when macroscopic water is dispersed into micron-sized droplets, either due to the uniform orientation of the dipole structure of water molecules or due to the double electrical layer structure formed on its surface, a 10 9 V / m electric field, such a strong electric field will tear the hydroxide in the water into hydroxyl free radicals ( ● OH) and electrons (e - ). Among them, hydroxyl radicals can trigger oxidation reactions, electrons can trigger reduction reactions, and electric fields can catalyze chemical reactions, making microdroplets a reactor for rapid chemical derivatization and small-scale synthesis. Since the flight speed of microdroplets is generally tens of meters per second, up to nearly 100 meters per second, and the droplet size is only a few microns, it is difficult to collect such high-speed flying and small droplets. At present, there is no technology that can achieve efficient collection of high-speed flying microdroplets.

[0003] It should be noted that the information disclosed in the above background technology section is only used to enhance the understanding of the background of the present disclosure, and therefore may include information that does not constitute the prior art known to ordinary technicians in the field. Summary of the invention

[0004] The present invention aims to provide a micro-droplet generation and collection device to solve the technical problems in the current micro-droplet chemistry field. The device can efficiently collect micro-droplets while ensuring the size and uniformity of the micro-droplets.

[0005] First, the present invention provides a micro-droplet generation and collection device, which adopts the following technical scheme: including a -80℃ refrigeration system, a micro-droplet preparation system and a collection system. The -80℃ refrigeration system is a -80℃ cooling circulation pump, and the liquid outlet pipe and the liquid inlet pipe of the -80℃ cooling circulation pump are respectively inserted into the condensate inlet and the condensate outlet of the collection system, and the condensate only flows through the serpentine condenser of the collection system. The micro-droplet preparation system consists of a carrier gas device, a three-way pipe fitting and an injection pump. One end of the two ends of the same straight line of the three-way pipe fitting is connected by a threaded manner to a first peek tube with an inner diameter of 0.2mm and no fixed outer diameter requirement, which only needs to be tightly connected with the threaded plug. The port is the micro-droplet generation site, and the other end is threaded to penetrate the fused silica capillary with an inner diameter of 0.1mm and an outer diameter of 0.192mm to the micro-droplet generation end of the three-way pipe fitting, and the vertical interface is connected to the carrier gas pipeline in a threaded manner. One end of the fused quartz tube inserted into the tee is connected to a second peek tube with an inner diameter of 0.192 mm and an outer diameter of 1.59 mm, and the second peek tube is tightly connected to the two-way through a threaded plug. The other end of the two-way is threadedly connected to a third peek tube with an inner diameter of 0.75 mm and an outer diameter of 1.59 mm. A micro-syringe can be inserted into the third peek tube, and the micro-syringe is pushed by the injection pump to transport the liquid into the fused quartz capillary, and is broken up into micro-droplets by high-pressure gas at the outlet. The collection system is a U-shaped glass device with a high left end and a low right end, wherein the middle part is a serpentine condenser, wherein the serpentine glass tube inside the serpentine condenser is integrally formed with the micro-droplet blowing end on the left, the liquid taking port at the bottom of the serpentine condenser and the gas outlet on the right, wherein the micro-droplet blowing end is a cylindrical glass tube of a certain length, wherein a polytetrafluoroethylene threaded plug is installed on the upper part thereof, wherein one or more small holes of a certain size are reserved for the polytetrafluoroethylene threaded plug, wherein the liquid taking port at the bottom is installed with a polytetrafluoroethylene threaded plug, and a frosted glass plug can be installed on the gas outlet on the right side, and the gas outlet faces the upper left side. The micro-droplet generating device is inserted into the collection system, and the carrier gas with micro-droplets flows through the micro-droplet blowing port and is frozen in the serpentine condenser, thereby realizing the preparation and collection of micro-droplets.

[0006] The collecting system is a U-shaped glass device with a high left end and a low right end, and the middle part is a serpentine condenser.

[0007] The serpentine glass tube inside the serpentine condenser is connected to the micro-droplet blowing end on the left, the liquid collection port at the bottom of the serpentine condenser and the gas outlet on the right. The liquid collection port is at the bottom of the serpentine condenser of the collection system and is inclined at a certain angle to better collect the liquid.

[0008] The serpentine glass tube inside the serpentine condenser is connected to the micro-droplet blowing end on the left, the liquid intake port at the bottom of the serpentine condenser and the gas outlet on the right. The micro-droplet blowing end is a cylindrical glass tube with a certain length, a polytetrafluoroethylene threaded plug is installed on the upper part, and the polytetrafluoroethylene threaded plug is reserved with one or more small holes of a certain size. The liquid intake port at the bottom is installed with a polytetrafluoroethylene threaded plug, and the gas outlet on the right is installed with a frosted glass plug, and the gas outlet faces the upper left side.

[0009] The liquid inlet is located at the bottom of the serpentine condenser tube of the collection system and is inclined at a certain angle.

[0010] Secondly, the present invention provides a method for generating and collecting microdroplets by the above device, comprising the following steps:

[0011] Step S1, start the refrigeration system, connect the pipeline, and wait until it reaches -80°C;

[0012] Step S2, start the carrier gas to remove moisture from the instrument;

[0013] Step S3, start the refrigeration cycle and wait for the instrument to cool down to below -50°C;

[0014] Step S4, starting the microinjection pump to prepare microdroplets;

[0015] Step S5, closing the carrier gas and the gas outlet, and collecting the micro-droplets after returning to room temperature.

[0016] In the method of the present invention, the size of the generated micro-droplets is achieved by adjusting the pressure of the carrier gas.

[0017] The advantages of the present invention are simple structure, convenient operation, and can realize efficient collection of micro-droplets, and can be used for amplified experiments of micro-droplet reactions, and has high application value; since the micro-droplet reaction only takes tens to hundreds of microseconds, the left part of the collection system of the device leaves enough reaction time for the micro-droplet reaction, so the lower temperature of the condensate cannot affect the reaction rate of the reaction in the micro-droplets; the tetrafluoroethylene threaded plug on the left side of the collection system is expandable, and multiple micro-droplet generation devices can be integrated at the same time, thereby improving the generation efficiency of the micro-droplets. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 A flow chart of the use of a micro droplet generation and collection device

[0019] Figure 2 Schematic diagram of a microdroplet preparation system.

[0020] Figure 3 Schematic diagram of a micro-droplet collection system.

[0021] Figure 4It is a schematic diagram of a micro-droplet generation and collection device.

[0022] In the figure: 1. carrier gas pipeline; 2. three-way pipe fitting; 3. injection pump; 4. first peek tube; 5. fused silica capillary; 6. second peek tube; 7. two-way; 8. third peek tube; 9. micro syringe; 10. serpentine condenser; 11. gas outlet; 12. cylindrical glass tube; 13. polytetrafluoroethylene threaded plug; 14. liquid collection port; 15. -80℃ cooling circulation pump; 16. liquid outlet pipe; 17. liquid inlet pipe; 18. condensate inlet; 19. condensate outlet. DETAILED DESCRIPTION

[0023] To make the purpose, technical solution and advantages of the embodiments of the present disclosure clearer, the technical solution of the embodiments of the present disclosure will be described clearly and completely below. If no specific conditions are specified in the embodiments, the conventional conditions or the conditions recommended by the manufacturer shall be followed.

[0024] A micro-droplet generating and collecting device is further described in detail below in conjunction with the accompanying drawings.

[0025] See attached Figure 1 The present invention provides a method for using a micro-droplet generation and collection device, comprising:

[0026] Step S1, start the refrigeration system, connect the pipeline, and wait until it reaches -80°C;

[0027] Step S2, start the carrier gas to remove moisture from the instrument;

[0028] Step S3, start the refrigeration cycle and wait for the instrument to cool down to below -50°C;

[0029] Step S4, starting the microinjection pump to prepare microdroplets;

[0030] Step S5, closing the carrier gas and the gas outlet, and collecting the micro-droplets after returning to room temperature.

[0031] The micro-droplet preparation method can control the size of the generated micro-droplets by adjusting the pressure of the carrier gas.

[0032] like Figure 2As shown, a schematic diagram of a micro-droplet preparation system described in the present invention: the micro-droplet preparation system consists of a gas carrier device, a three-way pipe fitting 2 and a syringe pump 3. The gas carrier device is connected to the gas carrier pipeline 1 of the three-way pipe fitting 2. The two ends of the same straight line of the three-way pipe fitting 2 are connected to the first peek tube 4 with an inner diameter of 0.2 mm and no fixed outer diameter requirement, which only needs to be tightly connected with the threaded plug, in a threaded manner at one end, and the port is the micro-droplet generation end. The other end is threaded to penetrate the fused silica capillary 5 with an inner diameter of 0.1 mm and an outer diameter of 0.192 mm to the micro-droplet generation end of the three-way pipe fitting 2, and the vertical interface is connected to the gas carrier pipeline 1 in a threaded manner. One end of the fused silica capillary 5 inserted into the three-way pipe fitting 2 is connected to a second peek tube 6 with an inner diameter of 0.192 mm and an outer diameter of 1.59 mm, and the second peek tube 6 is tightly connected to one end of the two-way pipe fitting 7 through a threaded plug. The other end of the two-way pipe fitting 7 is threadedly connected to a third peek tube 8 with an inner diameter of 0.75 mm and an outer diameter of 1.59 mm. A micro-syringe 9 can be inserted into the third peek tube 8. The micro-syringe 9 is pushed by the injection pump 3 to transport the liquid into the fused silica capillary 5, and is broken up into micro-droplets by the high-pressure gas at the outlet.

[0033] like Figure 3 As shown, a schematic diagram of a micro-droplet collection system of the present invention is shown: the collection system is a U-shaped glass device with a high left end and a low right end, wherein the middle part is a serpentine condenser tube 10, the serpentine glass tube inside the serpentine condenser tube 10 is integrally formed with the micro-droplet blowing end on the left, the liquid taking port 14 at the bottom of the serpentine condenser tube 10 and the gas outlet 11 on the right, the micro-droplet blowing end is a cylindrical glass tube 12 of a certain length, the upper part of which is equipped with a polytetrafluoroethylene threaded plug 13, the polytetrafluoroethylene threaded plug 13 is reserved with one or more small holes of a certain size, the liquid taking port 14 at the bottom is equipped with a polytetrafluoroethylene threaded plug, the gas outlet 11 on the right can be equipped with a frosted glass plug, and the gas outlet faces the upper left side. The micro-droplet generating device is inserted into the collection system, and the carrier gas with micro-droplets flows through the micro-droplet blowing port and is frozen in the serpentine condenser tube 10, so as to realize the collection and preparation of micro-droplets.

[0034] like Figure 4 As shown, a micro-droplet generation and collection device described in the present invention includes a -80°C refrigeration system, a micro-droplet preparation system and a collection system. The -80°C refrigeration system is a -80°C cooling circulation pump 15, and the liquid outlet pipe 16 and the liquid inlet pipe 17 of the -80°C cooling circulation pump 15 are respectively inserted into the condensate inlet 18 and the condensate outlet 19 of the collection system. The first peek tube 4 at the micro-droplet generation end is inserted into the small hole reserved by the polytetrafluoroethylene threaded plug 13, and the micro-injection syringe 9 is connected to the two-way 7.

[0035] Turn on the refrigeration system and wait for the refrigerant to reach -80℃.

[0036] Remove the glass plug of the gas outlet 11. In order to avoid the influence of air moisture inside the instrument on the micro-droplet reaction, the carrier gas pipeline 1 connected to the carrier gas device should be opened before the micro-droplet preparation device is turned on to remove the moisture inside the instrument.

[0037] Turn on the refrigeration system refrigeration cycle. Due to the high temperature of the collection system, the coolant temperature will rise. In order to achieve better micro-droplet collection, you need to wait for the coolant temperature to drop below -50℃ and stabilize before continuing to the next step.

[0038] The injection pump 3 is turned on, and liquid is injected into the fused silica capillary 5 through the micro-injector 9. At this time, the micro-droplet preparation device starts to prepare micro-droplets, and the generated micro-droplets are carried by the carrier gas into the serpentine condenser 10 of the collection system. The temperature of the serpentine condenser 10 is as low as -50°C, and the micro-droplets brought into the serpentine condenser 10 by the carrier gas will be quickly frozen, thereby realizing the collection of micro-droplets.

[0039] After the micro-droplets are collected, the carrier gas pipeline 1 and the gas outlet 11 of the serpentine condenser 10 are quickly closed to prevent the frozen micro-droplets from volatilizing. Then the refrigeration system is turned off, and the collection system is waited to return to room temperature, and the liquid collection port (14) is opened to recover the collected micro-droplets.

[0040] Based on the above description, the present invention passes the fused silica capillary through the three-way pipe fitting, and pushes the microinjection needle piston to inject liquid into it through the injection pump, and the high-pressure carrier gas connected to the vertical interface of the three-way pipe fitting breaks up the droplets into micro-droplets; the micro-droplets are collected through a U-shaped serpentine condenser. The present invention cleverly integrates the micro-droplet generating device and the collecting device into one device, so that the device has a simple structure and is easy to operate, and can achieve ultra-high efficiency micro-droplet collection, which has high application value.

[0041] It should be further explained that the above implementation modes are only used to understand the technical solution of the present invention, and are not used to limit the protection scope of the present invention. Any obvious adjustments and modifications made to the technical solution of the present invention that belong to the technical concept of the present invention should also fall within the protection scope of the present invention.

Claims

1. A micro-droplet generating and collecting device, characterized in that: The invention comprises a -80°C refrigeration system, a micro-droplet preparation system and a collection system. The liquid outlet pipe (16) and the liquid inlet pipe (17) of the -80°C refrigeration system are respectively inserted into the condensate inlet (18) and the condensate outlet (19) of the collection system. The condensate only flows through the serpentine condenser (10) in the middle of the collection system. The serpentine glass tube inside the serpentine condenser (10) is connected with the micro-droplet blowing end on the left, the liquid taking port (14) at the bottom and the gas outlet (11) on the right. The micro-droplet blowing end is a cylindrical glass tube (12) of a certain length, and a polytetrafluoroethylene threaded plug (13) is installed on the upper part thereof. ), the polytetrafluoroethylene threaded plug (13) is reserved with one or more small holes of a certain size, the bottom liquid intake port (14) is installed with a polytetrafluoroethylene threaded plug, the right gas outlet (11) is installed with a frosted glass plug, and its outlet faces the upper left side, the first peek tube (4) at the micro-droplet generating end is inserted into the small hole reserved in the polytetrafluoroethylene threaded plug (13) at the micro-droplet blowing end of the collection system, the carrier gas pipeline (1) at the vertical end of the three-way pipe fitting (2) is connected to the high-pressure carrier gas, and the generated droplets flow through the micro-droplet blowing end, the serpentine tube of the serpentine condenser (10) and the gas outlet along with the connected carrier gas.

2. A micro-droplet generating and collecting device according to claim 1, characterized in that: The micro-droplet preparation system is composed of a gas carrier device, a three-way pipe fitting (2) and a syringe pump (3). One of the two ends of the same straight line of the three-way pipe fitting (2) is connected to the micro-droplet generation end of a first peek tube (4) with an inner diameter of 0.2 mm in a threaded manner, and the other end is threaded to penetrate a fused silica capillary (5) with an inner diameter of 0.1 mm and an outer diameter of 0.192 mm into the micro-droplet generation end of the three-way pipe fitting (2). The vertical interface is connected to the gas carrier pipeline (1) in a threaded manner.

3. A micro-droplet generating and collecting device according to claim 1, characterized in that: The two ends of the fused silica capillary (5) are connected to a second peek tube (6) with an outer diameter of 1.59 mm. The second peek tube (6) is tightly connected to a peek threaded plug. The peek threaded plug at one end is connected to one end of a two-way (7). The other end of the two-way (7) is threadedly connected to a third peek tube (8) with an inner diameter of 0.75 mm and an outer diameter of 1.59 mm. A micro-syringe (9) can be inserted into the third peek tube (8).

4. A micro-droplet generating and collecting device according to claim 1, characterized in that: The injection pump (3) injects the liquid into the fused silica capillary (5) via the micro-injector (9).

5. A micro-droplet generating and collecting device according to claim 1, characterized in that: The -80°C refrigeration system is a -80°C cooling circulation pump (15), the liquid outlet (16) and liquid inlet (17) of the -80°C cooling circulation pump (15) are respectively connected to the condensate inlet (18) and condensate outlet (19) of the collection system through an insulating pipe, and the condensate only flows through the part of the serpentine condenser (10) in the middle of the collection system.

6. A micro-droplet generating and collecting device according to claim 1, characterized in that: The collecting system is a U-shaped glass device with a high left end and a low right end, and the middle part is a serpentine condenser (10).

7. A micro-droplet generating and collecting device according to claim 1, characterized in that: The serpentine glass tube inside the serpentine condenser (10) is connected to the micro-droplet blowing end on the left, the liquid intake port (14) at the bottom of the serpentine condenser (10) and the gas outlet (11) on the right. The micro-droplet blowing end is a cylindrical glass tube (12) of a certain length, on the upper part of which a polytetrafluoroethylene threaded plug (13) is installed, and the polytetrafluoroethylene threaded plug (13) is reserved with one or more small holes of a certain size. The liquid intake port (14) at the bottom is installed with a polytetrafluoroethylene threaded plug, and the gas outlet (11) on the right is installed with a frosted glass plug, and the gas outlet (11) faces the upper left side.

8. A micro-droplet generating and collecting device according to claim 1, characterized in that: The liquid inlet (14) is located at the bottom of the serpentine condenser tube (10) of the collection system and is inclined at a certain angle.

9. A method for generating and collecting microdroplets, implemented by the device according to any one of claims 1 to 8, characterized in that The following steps are involved: Step S1, start the refrigeration system, connect the pipeline, and wait until it reaches -80°C; Step S2, start the carrier gas to remove moisture from the instrument; Step S3, start the refrigeration cycle and wait for the instrument to cool down to below -50°C; Step S4, starting the microinjection pump to prepare microdroplets; Step S5, closing the carrier gas and the gas outlet, and collecting the microdroplets after returning to room temperature.

10. The method for generating and collecting microdroplets according to claim 9, characterized in that: The size of the generated microdroplets is achieved by adjusting the pressure of the carrier gas.

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