A device for electro-droplet reaction and product collection

Abstract

The present invention proposes a device for electro-droplet reaction and product collection, which includes an air chamber, a counter electrode, a sample tray, a capillary and a cover plate, wherein a cover plate is provided above the tip of the capillary in a controllable gas environment provided by the air chamber, and its inner surface is designed to be a dome-shaped structure for condensing the droplets formed by electrospray and guiding the droplets to flow back to the sample tray, thereby reducing interference with the spray operation. This circulation reflux design allows the unreacted components to be recovered, continue to be sprayed through the capillary, and circulate to participate in the reaction process, thereby significantly improving the reaction efficiency. The device has a simple structure, high stability, and a wide range of applications. It provides an efficient and reliable droplet synthesis technology platform for chemical synthesis experiments and industrial production, effectively improving the efficiency and quality of chemical synthesis, and is of great significance for expanding the application scenarios of chemical synthesis.

Description

Technical Field

[0001] The present invention relates to the field of chemical synthesis devices, in particular to a device for electric droplet reaction and product collection. Background Art

[0002] Electrospray technology has been widely used in analytical chemistry, mass spectrometry, and chemical reactions, and has particularly significant advantages in microdroplet reaction technology for organic synthesis. This technology significantly accelerates reaction rates and improves reaction efficiency by applying a high-voltage electric field to form a stable microdroplet spray from a solution. However, traditional electrospray reaction devices have certain limitations when collecting microdroplet reaction products, such as the difficulty in efficiently condensing and refluxing the droplets and the high waste of unreacted products. In addition, current devices do not provide effective solutions for the introduction of gaseous reactants and the control of the reaction atmosphere, which limits the applicability and flexibility of the reaction.

[0003] Existing electrospray devices are primarily used for analytical testing, while devices that integrate reaction and product collection functions are still lacking. In the field of organic chemical synthesis, achieving efficient and stable spray reactions while ensuring product recovery and flexible control of the gas environment has become a key and challenging area of ​​technical research.

[0004] It should be noted that the information disclosed in the above background technology section is only used to understand the background of this application, and therefore may include information that does not constitute prior art known to ordinary technicians in this field. Summary of the Invention

[0005] The main purpose of the present invention is to overcome the defects existing in the above-mentioned background technology and provide a device for electro-droplet reaction and product collection.

[0006] To achieve the above object, the present invention adopts the following technical solutions:

[0007] A device for electro-droplet reaction and product collection, comprising:

[0008] A gas chamber, used to provide a controllable gas atmosphere or serve as a passage for gaseous reactants, is provided with a lower gas inlet and an upper gas outlet for gas input and discharge to regulate the gas environment in the gas chamber;

[0009] The counter electrode, wherein the lower electrode is located at the bottom of the sample tray and the upper electrode is located on the upper side of the cover plate, generates a potential difference by applying a high voltage to charge the solution;

[0010] a sample tray for carrying a reaction sample mixed solution;

[0011] at least one capillary tube, the bottom end of which is inserted below the liquid level of the solution in the sample tray, and the electrospray is formed through the tip of the capillary tube;

[0012] A cover plate is arranged above the capillary and is used for condensing droplets formed by electrospray and guiding the droplets to drip back to the sample plate along the intersection edge of the dome-shaped structure on the inner surface of the cover plate.

[0013] Further:

[0014] The dome-shaped structure of the inner surface of the cover plate may be in the form of an arch or a triangle.

[0015] The inner surface of the cover plate includes a plurality of dome-shaped structures, and the tip of each capillary tube corresponds to the center of each dome-shaped structure.

[0016] The outer diameter of the capillary is no greater than 1.5 mm, and the inner diameter is no greater than 800 μm.

[0017] The inner diameter of the spray emission tip of the capillary is no more than 150 μm, and the total length is no more than 70 mm.

[0018] The distance between the tip of the capillary tube and the inner surface of the cover plate is no more than 50 mm.

[0019] The bottom end of the capillary tube is below the liquid surface and does not contact the bottom of the sample tray.

[0020] Material choices for the capillary include quartz, glass, or metal.

[0021] The effective range of the electrodes covers the range of electrospray.

[0022] The sample tray is a columnar hollow liquid-carrying groove.

[0023] The sample tray is designed to be a heating or cooling structure to further regulate the reaction temperature.

[0024] The present invention has the following beneficial effects:

[0025] The present invention provides a device for electro-micro-droplet reaction and product collection, which is particularly suitable for the micro-droplet electrospray reaction system in organic chemistry, and can efficiently realize the collection of reaction products and the recycling of unreacted components. In the present invention, a controllable gas atmosphere or a channel for gaseous reactants is provided by an air chamber. In the controlled gas environment provided by the air chamber, a cover plate is provided above the capillary, and the inner surface of the cover plate is designed with a dome-shaped structure. The droplets formed by condensation are guided to the intersection edge of the dome-shaped structure and smoothly drip back to the sample tray. This design significantly improves the efficiency of electro-micro-droplet reaction and product collection. The dome-shaped structure of the cover plate not only optimizes the condensation process, but also realizes effective drainage and reflux of the droplets. Through this design, the droplets formed by condensation on the inner surface of the cover plate are guided to the intersection edge of the dome-shaped structure and smoothly drip back to the reflux mechanism of the sample tray, ensuring that the droplets can re-participate in the reaction system, reducing interference with the capillary spray operation, and significantly improving the reaction efficiency. Furthermore, the design of multiple dome-shaped structures, with each capillary tip corresponding to the center of the dome, further enhances the efficiency of condensation and reflux, ensuring the uniformity and continuity of the reaction.

[0026] The embodiments of the present invention have the following advantages:

[0027] First, through the design of the electrode high-voltage electric field and the capillary self-priming spray structure, the continuity of electrospray without pump drive is achieved, and the reaction uniformity is also improved.

[0028] Secondly, the dome-shaped cover design on the inner surface significantly improves the condensation efficiency, ensuring that the droplets quickly flow back to the sample tray and avoiding interference with the spray.

[0029] Third, the gas chamber design supports operation in a controllable gas environment, can input gaseous reactants and adjust temperature and humidity, expanding the scope of application of the reaction.

[0030] Finally, the reflux system is used to achieve the recycling of unreacted components, greatly improving the reaction efficiency and reducing resource waste.

[0031] Overall, the present invention, through its unique cover plate design, not only improves condensation efficiency and reaction uniformity, but also achieves the recycling of unreacted components and reduces resource waste, thereby providing an efficient and reliable droplet synthesis technology platform with a simple structure, high stability, and a wide range of applications, significantly improving the efficiency and quality of laboratory and industrial synthesis reactions.

[0032] The present invention is suitable for rapid and efficient application in organic chemical synthesis, drug development and industrial chemical reactions.

[0033] Other beneficial effects of the embodiments of the present invention will be further described below. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 This is a schematic structural diagram of an electro-droplet reaction and product collection device in the first embodiment of the present invention;

[0035] The numbers in the figure are 1, counter electrode, 2, sample plate, 3, capillary, 4, cover plate, 5, gas chamber, 6, reaction sample solution, 7, air inlet, and 8, air outlet. DETAILED DESCRIPTION

[0036] The following is a detailed description of the embodiments of the present invention. It should be emphasized that the following description is only exemplary and is not intended to limit the scope of the present invention and its application.

[0037] It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it can be directly on the other element or indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or indirectly connected to the other element. In addition, connection can be used for both fixing and coupling or communication.

[0038] It should be understood that the terms "length", "width", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the embodiments of the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation, and therefore cannot be understood as limiting the present invention.

[0039] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of such features. In the description of the embodiments of the present invention, "plurality" means two or more, unless otherwise specifically defined.

[0040] The present invention provides an efficient and stable electrospray droplet reaction and product collection device, aiming to solve the problems of unstable spraying, low product collection efficiency and insufficient control of reaction conditions in existing electrospray reaction devices.

[0041] See Figure 1The device for electro-droplet reaction and product collection according to an embodiment of the present invention includes: a gas chamber 5 for providing a controllable gas atmosphere or serving as a passage for gaseous reactants, and having a lower gas inlet 7 and an upper gas outlet 8 for gas input and output to regulate the gas environment within the gas chamber 5; a counter electrode 1, wherein the lower electrode 1 is located at the bottom of the sample tray 2 and the upper electrode 1 is located on the upper side of the cover plate 4, and a potential difference is generated by applying a high voltage to charge the solution; a sample tray 2 for holding a reaction sample solution 6; at least one capillary 3, the bottom end of which is inserted below the liquid level of the reaction sample solution 6 in the sample tray 2, and an electrospray is formed through the tip of the capillary 3; a cover plate 4, which is disposed above the capillary 3 and is used to condense droplets formed by the electrospray and guide the droplets to drip back to the sample tray 2 along the intersection edge of the dome-shaped structure on the inner surface of the cover plate 4. The dome-shaped structure on the inner surface of the cover plate 4 includes, but is not limited to, an arch or a triangle. Preferably, the inner surface of the cover plate 4 includes a plurality of dome-shaped structures, and the tip of each capillary tube 3 corresponds to the center of each dome-shaped structure.

[0042] The device according to the present invention features a cover plate 4 positioned above the capillary tube 3 within the controlled gas environment provided by the gas chamber 5. The inner surface of the cover plate 4 features a dome-shaped design. This inner surface serves to condense droplets formed by the spray and direct them along the intersecting edges of the dome structure into the sample tray 2, ensuring that the droplets flow back into the reaction system and minimizing interference with the spraying operation of the capillary tube 3. This circulatory reflux design allows unreacted components to condense and flow back into the sample tray 2, while the capillary tube 3 continues spraying, circulating in the reaction process and significantly improving reaction efficiency.

[0043] Therefore, the present invention provides an electric droplet reaction device that can integrate reaction, condensation, reflux and atmosphere control. Through its structural optimization and functional integration, the efficiency and applicability of droplet reaction are significantly improved. The device has the advantages of simple structure, high stability and wide range of applicability. It is an efficient and reliable droplet synthesis technology platform that can significantly improve the efficiency and quality of laboratory and industrial synthesis reactions, effectively meeting the needs of chemical synthesis experiments and industrial production, and is of great significance for improving chemical synthesis efficiency and expanding application scenarios.

[0044] Specific embodiments of the present invention are further described below.

[0045] An electro-droplet reaction and product collection device comprises: a counter electrode 1, a sample tray 2, a capillary 3, a cover plate 4 and an air chamber 5. The air chamber 5 is used to provide a controllable gas environment or serve as a channel for gaseous reactants. The air chamber 5 is designed with a lower air inlet 7 and an upper air outlet 8 for inputting or discharging gas to achieve precise control of the gas atmosphere, adapt to different reaction conditions, and form a continuous reaction process. The air chamber 5 can adjust the temperature or humidity to meet the needs of different chemical reactions. By applying a high voltage to the counter electrode 1, a potential difference is generated at the bottom of the sample tray 2, so that the reaction sample solution 6 is charged, and a stable electrospray is generated through the tip of the capillary 3. The sample tray 2 is used to carry the reaction sample solution 6 and is designed to be heated or cooled. The reaction temperature can be further controlled to meet diverse reaction conditions. The bottom end of the capillary 3 spray system is inserted into the reaction sample solution 6, and the reaction sample solution 6 is sucked to the tip by capillary force. A high voltage is applied to achieve a stable spray process, and the stability of the spray and the reaction efficiency are improved by controlling the distance between the spray emission tip and the cover plate 4. The inner surface of the cover plate 4 with a dome-shaped inner surface is used to condense the droplets formed by the spray, and the droplets are drained into the sample tray 2 along the intersection edge of the dome-shaped structure to ensure that the droplets flow back to the reaction system, reducing interference with the spray operation of the capillary 3. The circulation reflux design allows the unreacted components to flow back to the sample tray 2 after condensation, and the capillary 3 continues to spray, circulating in the reaction process, significantly improving the reaction efficiency.

[0046] The specific working process is as follows: the reaction sample solution 6 is added to the sample tray 2, and the solution temperature is adjusted by heating or cooling as needed. The capillary 3 draws the solution from the sample tray 2 to the spray tip, and at the same time adjusts the gas environment through the gas chamber 5 to meet the reaction conditions. Subsequently, high voltage is applied to the electrode 1 system to charge the solution, and a stable electrospray is generated through the tip of the capillary 3. After the spray droplets condense on the inner surface of the dome-shaped structure of the cover plate 4, they flow back to the sample tray 2 along the intersection edge, and the unreacted components are recycled and continue to participate in the reaction process. The reaction products gradually accumulate in the sample tray 2, and the product solution is finally collected and processed, thereby achieving efficient completion of the reaction and full recovery of the products.

[0047] In some embodiments, the counter electrode 1 is placed on the bottom of the sample tray 2 and the upper side of the cover plate 4 in any form including but not limited to embedding, splicing, etc. The electrode 1 can be made of various conductive materials such as metal and graphite. Without considering the cost, materials with good conductivity are preferably used, such as precious metals such as gold, platinum, and silver.

[0048] In some embodiments, the dome-shaped structure of the inner surface of the cover plate 4 can be an arch, a triangle, etc. but is not limited to any form. Furthermore, the inner surface of the cover plate 4 is smooth and free of burrs.

[0049] In some embodiments, the capillary tube 3 can be made of various materials with an outer diameter of no more than 1.5 mm and an inner diameter of no more than 800 μm; the inner diameter of the spray emission tip of the capillary tube 3 is no more than 150 μm, and the total length is no more than 70 mm; further, the capillary tube 3 can be made of different materials such as quartz, glass, and metal; further, the distance between the tip of the capillary tube 3 and the inner surface of the cover plate 4 is no more than 50 mm; further, the bottom end of the capillary tube 3 is below the liquid level and does not contact the bottom of the sample tray 2;

[0050] In some embodiments, the sample tray 2 can be a hollow columnar liquid-carrying groove of various shapes and can be designed to be heated or cooled to further control the reaction temperature and meet diverse reaction conditions. The reaction sample solution 6 in the sample tray 2 needs to be a conductive liquid.

[0051] By applying a high voltage to the counter electrode 1, a potential difference is generated at the bottom of the sample tray 2, so that the reaction sample solution 6 is charged, and an electrospray is stably generated through the tip of the capillary 3. The spray condenses after hitting the inner surface of the cover plate 4, and flows back to the sample tray 2 along the intersection edge of the dome-shaped structure on the inner surface of the cover plate 4, effectively avoiding interference with the capillary 3 spray needle operation, and improving the stability and reaction efficiency of the spray. The design of the gas chamber 5 enables the device to operate in a controllable gas environment, or introduce gaseous reactants, further expanding the applicability and flexibility of the reaction. The device can efficiently collect reaction products, and the unreacted components reflux through the sample tray 2 and circulate into the reaction process, significantly improving the reaction efficiency and achieving rapid synthesis. The present invention has the advantages of simple structure, high reaction efficiency, and a wide range of applications, and is suitable for promotion and application in chemical synthesis experiments and industrial production.

[0052] Example 1

[0053] like Figure 1 As shown, an electrospray droplet reaction and product collection device comprises an air chamber 5, within which a sample tray 2 is positioned for holding a reaction solution. A capillary tube 3 is inserted below the liquid level of a reaction sample solution 6 in the sample tray, drawing the solution to the capillary tip via capillary action. A lower electrode 1 is positioned at the bottom of the sample tray 2, and an upper electrode 1 is positioned atop a cover plate 4. A high voltage is applied between the upper and lower electrodes to create a potential difference (ΔV), thereby generating an electrospray at the capillary tip. The cover plate 4, with a dome-shaped inner surface, is positioned above the capillary tube to condense the spray droplets and direct them to the sample tray. Air inlets 7 and outlets 8 are provided on either side of the air chamber for regulating the gas environment or introducing gaseous reactants, thereby meeting different reaction requirements. The sample tray can be equipped with a fixture, such as a bracket, to secure the position of the capillary tube 3. A flat electrode below the counter electrode 1 is positioned at the bottom of the sample tray, while an upper counter electrode is positioned flat on the upper side of the flat cover plate. Wires are then connected to each other to apply a high voltage between the counter electrodes, generating a potential difference.

[0054] The specific usage is as follows:

[0055] Place the lower electrode 1 of the counter electrode system at the bottom of the sample tray, fix the upper electrode 1 on the top of the cover plate, and connect it to the high-voltage power supply through a wire;

[0056] Add an appropriate amount of reaction sample solution 6 to the sample tray, and fix the capillary with a bracket so that its bottom is inserted below the liquid surface of the solution and aspirate the reaction sample solution 6 to the tip, avoiding contact with the bottom of the sample tray;

[0057] Place the fixed cover plate on the capillary, ensuring that the distance between the cover plate and the capillary tip does not exceed 70 mm;

[0058] The entire device is placed in the gas chamber, and the gas environment inside the gas chamber is adjusted through the gas inlet 7 and the gas outlet 8, and the gaseous reactants are introduced or the gas composition is maintained constant according to the needs;

[0059] Start the high-voltage power supply and apply high voltage to the upper and lower electrodes to form a potential difference, so that a stable electrospray is generated at the capillary tip;

[0060] The ejected droplets condense on the inner surface of the dome-shaped cover plate and then flow back to the sample tray through the intersecting edges;

[0061] Place one of the counter electrodes 1 connected to the wire on the bottom of the sample tray, and the other counter electrode on the cover;

[0062] The unreacted components in the droplets that flow back to the sample plate can be reabsorbed through the capillary and enter the spray process, thus forming a highly efficient circular reaction;

[0063] After multiple cycles of reaction, the products gradually accumulate in the sample tray and can be collected by sampling or separation methods.

[0064] This device significantly improves electrospray stability, reaction efficiency, and product collection rate through the controlled gas environment of the gas chamber, the high-voltage electric field between the upper and lower electrodes, and the condensation and reflux design of the dome-shaped inner cover. Unreacted components are reused repeatedly through a circulation system, reducing resource waste and further optimizing the reaction process. This device is suitable for both laboratory and industrial organic chemical synthesis, enabling efficient and rapid synthesis reactions while ensuring easy operation and flexible control of reaction conditions, providing a reliable technical platform for chemical research and industrial applications.

[0065] The above description further details the present invention in conjunction with specific / preferred embodiments, and the specific implementation of the present invention should not be construed as being limited to these descriptions. Persons skilled in the art will appreciate that, without departing from the spirit of the present invention, they may make various substitutions or modifications to the described embodiments, and these substitutions or modifications should be considered to fall within the scope of protection of the present invention. Throughout this specification, reference to terms such as "one embodiment," "some embodiments," "preferred embodiments," "examples," "specific examples," or "some examples" indicates that the specific features, structures, materials, or characteristics described in conjunction with such embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of these 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 any one or more embodiments or examples. Persons skilled in the art may combine and assemble the different embodiments or examples described in this specification, as well as features of different embodiments or examples, without conflicting opinions. Although the embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions, and modifications may be made herein without departing from the scope of protection of the patent application.

Claims

1. A device for electro-droplet reaction and product collection, characterized in that: include: A gas chamber, used to provide a controllable gas atmosphere or serve as a passage for gaseous reactants, is provided with a lower gas inlet and an upper gas outlet for gas input and discharge to regulate the gas environment in the gas chamber; a sample tray for carrying a reaction sample mixed solution; The counter electrode, wherein the lower electrode is located at the bottom of the sample tray and the upper electrode is located on the upper side of the cover plate, generates a potential difference by applying a high voltage to charge the solution; at least one capillary tube, the bottom end of which is inserted below the liquid level of the solution in the sample tray, and the electrospray is formed through the tip of the capillary tube; A cover plate is arranged above the capillary and is used for condensing droplets formed by electrospray and guiding the droplets to drip back to the sample plate along the intersection edge of the dome-shaped structure on the inner surface of the cover plate.

2. The device according to claim 1, characterized in that The dome-shaped structure of the inner surface of the cover plate may be in the form of an arch or a triangle.

3. The device according to claim 1 or 2, characterized in that The inner surface of the cover plate includes a plurality of dome-shaped structures, and the tip of each capillary tube corresponds to the center of each dome-shaped structure.

4. The device according to claim 1 or 2, characterized in that The outer diameter of the capillary is no greater than 1.5 mm, the inner diameter is no greater than 800 μm, the inner diameter of the spray emission tip of the capillary is no greater than 150 μm, and the total length is no greater than 70 mm.

5. The device according to claim 1 or 2, characterized in that The distance between the tip of the capillary tube and the inner surface of the cover plate is no more than 50 mm.

6. The device according to claim 1 or 2, characterized in that The bottom end of the capillary tube is below the liquid surface and does not contact the bottom of the sample tray.

7. The device according to claim 1 or 2, characterized in that Material choices for the capillary include quartz, glass, or metal.

8. The device according to claim 1 or 2, characterized in that The effective range of the electrodes covers the range of electrospray.

9. The device according to claim 1 or 2, characterized in that The sample tray is a columnar hollow liquid-carrying groove.

10. The device according to claim 1 or 2, characterized in that The sample tray is designed to be a heating or cooling structure to further regulate the reaction temperature.

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