Device for electric microdroplet reaction and product collection

Abstract

The invention provides a device for electric microdroplet reaction and product collection, the device comprises a gas chamber, a counter electrode, a sample disc, a capillary tube and a cover plate, in a controllable gas environment provided by the gas chamber, the cover plate is arranged above the tip end of the capillary tube, the inner surface of the cover plate is designed into a dome-shaped structure, and the cover plate is used for condensing liquid droplets formed by electric spray; and the liquid drops are guided to flow back to the sample disc, so that interference on spraying operation is reduced. According to the circulating reflux design, unreacted components are recycled, are continuously sprayed through the capillary tubes and circularly participate in the reaction process, so that the reaction efficiency is remarkably improved. The device is simple in structure, high in stability and wide in application range, an efficient and reliable microdroplet synthesis technical platform is provided for chemical synthesis experiments and industrial production, the efficiency and quality of chemical synthesis are effectively improved, and the device has important significance for expanding the application scene of chemical synthesis.

Description

Technical Field

[0001] The 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 the fields of analytical chemistry, mass spectrometry and chemical reactions, especially in the micro-droplet reaction technology in organic synthesis. This technology can significantly accelerate the reaction rate and improve the reaction efficiency by applying a high-voltage electric field to form a stable micro-droplet spray from the solution. However, traditional electrospray reaction devices have certain limitations when collecting micro-droplet reaction products, such as the difficulty in efficiently condensing and refluxing the droplets and the large amount of unreacted products being wasted. In addition, current devices have not yet provided an effective solution 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 mostly used for analysis and detection, and devices that integrate reaction and product collection functions are not yet mature. Especially in the field of organic chemical synthesis, how to achieve efficient and stable spray reaction while ensuring product recycling and flexible regulation of the gas environment has become the focus and difficulty of technical research.

[0004] It should be noted that the information disclosed in the above background technology section is only used for understanding the background of the present application, and therefore may include information that does not constitute prior art known to ordinary technicians in the 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 inputting and discharging gas to adjust the gas environment in the gas chamber;

[0009] A counter electrode, wherein the lower electrode is located at the bottom of the sample plate and the upper electrode is located on the upper side of the cover plate, and a potential difference is generated 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, 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;

[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 each capillary tip 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 greater than 150 μm, and the total length is no greater than 70 mm.

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

[0019] The bottom end of the capillary 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 action range of the electrodes covers the range of electrospray.

[0022] The sample plate 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 is provided by an air chamber or as a channel for gaseous reactants. In the controllable gas environment provided by the air chamber, a cover plate is arranged above the capillary, and the inner surface of the cover plate is designed as 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 the 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, which ensures that the droplets can re-participate in the reaction system, reduces the interference with the capillary spray operation, and significantly improves 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 reaction efficiency and reducing resource waste.

[0031] In general, the present invention, through its unique cover plate design, not only improves the condensation efficiency and reaction uniformity, but also realizes 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, which significantly improves the efficiency and quality of laboratory and industrial synthesis reactions.

[0032] The 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 It 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, 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 and application of the present invention.

[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 fixing as well as for coupling or communication.

[0038] It should be understood that the orientation or position relationship indicated by terms such as "length", "width", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside" and "outside" 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 referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0039] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the embodiments of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and 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 spray, low product collection efficiency and insufficient control of reaction conditions existing in the existing electrospray reaction device.

[0041] See also Figure 1The device for electro-droplet reaction and product collection of the embodiment of the present invention comprises: a gas chamber 5 for providing a controllable gas atmosphere or serving as a passage for gaseous reactants, provided with a lower gas inlet 7 and an upper gas outlet 8 for inputting and discharging gas to adjust the gas environment in 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 carrying a reaction sample solution 6; at least one capillary 3, the bottom end of which is inserted below the liquid level of the solution 6 of the sample tray 2, and an electrospray is formed through the tip of the capillary 3; a cover plate 4, which is arranged above the capillary 3, for condensing droplets formed by the electrospray, and guiding 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] According to the device of the present invention, in the controllable gas environment provided by the gas chamber 5, a cover plate 4 is arranged above the capillary 3, and the inner surface of the cover plate 4 is designed as a dome-shaped structure. The inner surface of the cover plate 4 is used to condense the droplets formed by the spray, and guide the droplets along the intersection edge of the dome-shaped structure to the sample tray 2, ensuring that the droplets flow back to the reaction system, reducing interference with the spray operation of the capillary 3. Through this circulation reflux design, the unreacted components flow back to the sample tray 2 after condensation, and the capillary 3 continues to spray, and circulates to participate in the reaction process, significantly improving the 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 reactions are significantly improved. The device has the advantages of simple structure, high stability and wide application range. It is an efficient and reliable droplet synthesis technology platform, which can significantly improve the efficiency and quality of laboratory and industrial synthesis reactions, effectively meet the needs of chemical synthesis experiments and industrial production, and is of great significance for improving chemical synthesis efficiency and expanding application scenarios.

[0044] The 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 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. The counter electrode 1 generates a potential difference at the bottom of the sample tray 2 by applying a high voltage to the counter electrode 1, so that the 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 mixed solution 6, and is designed as a heating or cooling structure, which can further control the reaction temperature to meet diversified reaction conditions. The bottom end of the capillary 3 spray system capillary 3 is inserted into the sample solution 6, and the solution 6 is sucked to the tip by capillary force, and a high voltage is applied to achieve a stable spray process, and the stability and reaction efficiency of the spray 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 structure is used to condense the droplets formed by the spray, and guide the droplets along the intersection edge of the dome-shaped structure to the sample tray 2, ensuring that the droplets flow back to the reaction system, reducing interference with the spray operation of the capillary 3. The cyclic reflux design allows the unreacted components to flow back to the sample tray 2 after condensation, and the capillary 3 continues to spray and participate in the reaction process cyclically, significantly improving the reaction efficiency.

[0046] The specific working process is as follows: the reaction solution 6 is added to the sample tray 2, and the temperature of the solution 6 is adjusted by heating or cooling as required. The capillary 3 draws the solution 6 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, a high voltage is applied to the electrode 1 system to charge the solution 6, 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 finally the product solution 6 is 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 embedded, spliced, including but not limited to any form, and is placed on the bottom of the sample tray 2 and the upper side of the cover plate 4. The electrode 1 can be a conductive material of various materials such as metal and graphite. Regardless of cost, a material with good conductivity is preferred, 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., including but not limited to any other forms. Further, the inner surface of the cover plate 4 is smooth and free of burrs.

[0049] In some embodiments, the capillary 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 3 is no more than 150 μm, and the total length is no more than 70 mm; further, the capillary 3 can be made of different materials such as quartz, glass, metal, etc.; further, the distance between the tip of the capillary 3 and the inner surface of the cover plate 4 is no more than 50 mm; further, the bottom end of the capillary 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 may be a columnar hollow liquid-carrying groove of various shapes, and may be designed as a heating or cooling structure, which may further control the reaction temperature to meet various reaction conditions. The sample solution 6 in the sample tray 2 needs to be a conductive liquid.

[0051] By applying a high voltage to the electrode 1, a potential difference is generated at the bottom of the sample tray 2, the solution 6 is charged, and an electrospray is stably generated through the tip of the capillary 3. The spray condenses after touching 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] Embodiment 1

[0053] like Figure 1 As shown, an electro-droplet reaction and product collection device includes an air chamber 5, a sample tray 2 is arranged inside the air chamber for carrying a reaction solution; the root of a capillary 3 is inserted below the liquid level of a solution 6 in the sample tray, and the solution is sucked to the tip of the capillary by capillary action. The bottom of the sample tray 2 is provided with a lower electrode 1, and the top of the cover plate 4 is provided with an upper electrode 1. A high voltage is applied between the upper and lower electrodes to form a potential difference (ΔV), so that an electrospray is sprayed at the tip of the capillary. The cover plate 4 with a dome-shaped inner surface is arranged above the capillary for condensing the spray droplets and draining them to the sample tray. An air inlet 7 and an air outlet 8 are arranged on both sides of the air chamber for adjusting the gas environment or introducing gaseous reactants to meet different reaction requirements. The sample tray can be provided with a fixing device such as a bracket to fix the position of the inserted capillary 3; the flat electrode below the electrode 1 is selected to be placed at the bottom of the sample tray, and the flat electrode above is placed flat on the upper side of the flat cover plate, and then the wires are connected respectively to apply a high voltage to generate a potential difference between the electrodes.

[0054] The specific usage is as follows:

[0055] The lower electrode 1 of the counter electrode system is placed at the bottom of the sample tray, and the upper electrode 1 is fixed to the top of the cover plate and connected to a high voltage power supply through a wire;

[0056] Add an appropriate amount of reaction 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 the solution 6 is drawn to the tip, avoiding contact with the bottom of the sample tray;

[0057] Place the fixed cover plate on top of the capillary, making sure the distance between the cover plate and the tip of the capillary does not exceed 70 mm;

[0058] The whole 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 demand;

[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 tip of the capillary;

[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 pan, and place the other counter electrode on the cover plate;

[0062] The unreacted components in the droplets that flow back to the sample plate can be drawn again through the capillary and enter the spray process, thus forming an efficient cyclic 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 the stability, reaction efficiency and product collection rate of electrospray through the controllable gas environment of the gas chamber, the high-voltage electric field of the upper and lower electrodes, and the condensation and reflux design of the dome-shaped cover plate on the inner surface. The unreacted components are repeatedly used through the circulation system to reduce resource waste and further optimize the reaction process. The device is suitable for laboratory and industrial organic chemical synthesis, and can achieve efficient and rapid synthesis reactions. At the same time, it ensures that the equipment is easy to operate and the reaction conditions are flexibly controlled, providing a reliable technical platform for chemical research and industrial applications.

[0065] The above content is a further detailed description of the present invention in combination with specific / preferred embodiments, and it cannot be determined that the specific implementation of the present invention is limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, without departing from the concept of the present invention, it can also make several substitutions or modifications to these described embodiments, and these substitutions or modifications should be regarded as belonging to the protection scope of the present invention. In the description of this specification, the description of the reference terms "an embodiment", "some embodiments", "preferred embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials or characteristics described in combination with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily target the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner. In the absence of mutual contradiction, those skilled in the art can combine and combine the different embodiments or examples described in this specification and the features of different embodiments or examples. 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 can 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 inputting and discharging gas to adjust the gas environment in the gas chamber; A counter electrode, wherein the lower electrode is located at the bottom of the sample plate and the upper electrode is located on the upper side of the cover plate, and a potential difference is generated by applying a high voltage to charge the solution; A sample tray for carrying a reaction sample mixed solution; at least one capillary, 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; 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 each capillary tip corresponds to the center of each dome-shaped structure.

4. The device according to any one of claims 1 to 3, characterized in that The outer diameter of the capillary is not greater than 1.5 mm, the inner diameter is not greater than 800 μm, the inner diameter of the spray emission tip of the capillary is not greater than 150 μm, and the total length is not greater than 70 mm.

5. The device according to any one of claims 1 to 4, characterized in that: The distance between the tip of the capillary and the inner surface of the cover plate is no more than 50 mm.

6. The device according to any one of claims 1 to 5, characterized in that The bottom end of the capillary is below the liquid surface and does not contact the bottom of the sample tray.

7. The device according to any one of claims 1 to 6, characterized in that Material choices for the capillary include quartz, glass or metal.

8. The device according to any one of claims 1 to 7, characterized in that The action range of the electrodes covers the range of electrospray.

9. The device according to any one of claims 1 to 8, characterized in that The sample plate is a columnar hollow liquid-carrying groove.

10. The device according to any one of claims 1 to 9, 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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