Continuous flow microchannel reactor for ruthenium complex synthesis
By employing a serpentine microchannel reactor and a temperature detector in the synthesis of ruthenium complexes, the problems of low mass transfer efficiency and difficulty in temperature monitoring were solved, thus achieving high-quality synthesis of ruthenium complexes.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-12
- Publication Date
- 2026-03-31
AI Technical Summary
In existing technologies, the mass transfer efficiency of ruthenium complex synthesis is poor and the reaction temperature is difficult to monitor in real time, resulting in poor quality.
A continuous flow microchannel reactor is designed, employing a serpentine micronetwork channel tube and a temperature detector to enhance mass transfer efficiency and monitor the reaction temperature in real time.
By extending the residence time of reactants in the reactor and controlling the temperature in real time, the quality and consistency of ruthenium complexes were improved.
Smart Images
Figure CN224057343U_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the field of ruthenium complex reactor technology, specifically relating to a continuous flow microchannel reactor for the synthesis of ruthenium complexes. Background Technology
[0002] Ruthenium complexes are an important class of organometallic compounds. Their unique structure and good physicochemical properties make them potentially valuable in many fields. In the synthesis of ruthenium complexes, reactors are often used. Chemical reactors are mainly of the types of batch, continuous and semi-continuous operation reactors, each with different characteristics and applicable ranges.
[0003] Currently, when ruthenium, ligands, solvents, and inert gases react in a flask, the short residence time inside the flask results in poor mass transfer efficiency, and it is difficult to monitor the reaction temperature in real time. If the temperature is too low or too high, the quality of the ruthenium complex will be poor.
[0004] To address the above problems, this application designs a continuous flow microchannel reactor for the synthesis of ruthenium complexes, in order to solve the technical difficulties such as poor mass transfer efficiency and difficulty in real-time monitoring of the reaction temperature inside the flask, resulting in poor quality of ruthenium complexes. Utility Model Content
[0005] This application aims to address at least one of the technical problems existing in the prior art or related technologies.
[0006] Therefore, this application designs a continuous flow microchannel reactor for the synthesis of ruthenium complexes to improve mass transfer efficiency and monitor the reaction temperature inside the flask in real time to ensure the quality of the ruthenium complexes.
[0007] This application provides a continuous flow microchannel reactor for the synthesis of ruthenium complexes, comprising: a three-necked flask; a micro-network channel tube arranged in a serpentine shape inside the three-necked flask, with its inner wall coated with a corrosion-resistant material layer; a first neck tube connected to the upper left end of the three-necked flask; a microchannel feed assembly consisting of a feed pipe and a flow controller, located at the inlet of the first neck tube, for connecting and inputting ruthenium, ligands, solvent, and inert gas; a second neck tube connected to the middle of the upper end of the three-necked flask; a temperature detector and a temperature detection probe located at the inlet of the second neck tube, for real-time detection of the reaction temperature inside the three-necked flask; a third neck tube connected to the upper right end of the three-necked flask; and an outer bottle fitted over the three-necked flask, with a media flow channel between the three-necked flask and the outer bottle.
[0008] In some possible embodiments, the opening of the first neck tube is covered with a first sealing plug, the outlet of the microchannel feeding assembly is connected to a microchannel feeding tube, and the microchannel feeding tube extends through the first sealing plug into the first neck tube and the three-necked bottle, and the head end of the micro-network channel tube is connected to the end end of the microchannel feeding tube.
[0009] In some possible embodiments, a second sealing plug is provided at the opening of the second neck tube, one end of the temperature detector is connected to a temperature detection probe, and the temperature detection probe extends through the second sealing plug into the first neck tube and the three-necked bottle.
[0010] In some possible embodiments, the opening of the third neck tube is covered with a third sealing plug, and a microchannel outlet tube is provided inside the third neck tube. One end of the microchannel outlet tube is connected to the end of the micronetwork channel tube, and the microchannel outlet tube extends out of the third neck tube through the third sealing plug.
[0011] In some possible embodiments, the outer bottle has an inlet on one side and an outlet on the other side.
[0012] In some possible embodiments, the three-necked bottle is made of borosilicate glass.
[0013] In some possible embodiments, the other end of the microchannel outlet tube is connected to a serpentine cooling tube, the lower end of the serpentine cooling tube is connected to a reaction processor, and the lower end of the reaction processor is connected to a microprocessor.
[0014] Compared with the prior art, the technical solution provided in this application has at least the following beneficial effects:
[0015] This application provides a continuous flow microchannel reactor for the synthesis of ruthenium complexes. By arranging the micronetwork channel tubes in a serpentine pattern, a serpentine static mixing unit is formed, which helps to prolong the residence time of ruthenium, ligands, solvents, and inert gases in the three-necked flask. This enhances the mass transfer efficiency of ruthenium, ligands, solvents, and inert gases. Furthermore, by incorporating a temperature detector, the reaction temperature in the three-necked flask can be monitored in real time, thereby ensuring that the temperature is maintained between 20-150°C to prevent temperature runaway and effectively guarantee the quality of the ruthenium complexes.
[0016] Additional aspects and advantages of this application will become apparent in the following description or may be learned by practice of this application. Attached Figure Description
[0017] The above and / or additional aspects and advantages of this application will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which:
[0018] Figure 1 This is a schematic diagram of the overall structure of a continuous flow microchannel reactor for the synthesis of ruthenium complexes according to some embodiments of this application;
[0019] Figure 2 This is a schematic diagram of the internal structure of the first sealing plug of a continuous flow microchannel reactor for the synthesis of ruthenium complexes according to some embodiments of this application;
[0020] Figure 3 This is a schematic diagram of the internal structure of the second sealing plug of a continuous flow microchannel reactor for the synthesis of ruthenium complexes according to some embodiments of this application;
[0021] Figure 4 This is a schematic diagram of the internal structure of the third sealing plug of a continuous flow microchannel reactor for the synthesis of ruthenium complexes according to some embodiments of this application.
[0022] Figure label:
[0023] 1. Three-necked flask; 2. Microchannel tube; 3. First neck tube; 4. Second neck tube; 5. Third neck tube; 6. Microchannel feed assembly; 7. Microchannel feed tube; 8. Temperature detector; 9. Temperature detection probe; 10. Microchannel outlet tube; 11. Outer bottle; 12. Reaction processor; 13. Microprocessor; 14. Feed inlet; 15. Discharge outlet; 16. First sealing plug; 17. Second sealing plug; 18. Third sealing plug; 19. Serpentine cooling tube. Detailed Implementation
[0024] To better understand the above-mentioned objectives, features, and advantages of this application, the application will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be noted that, unless otherwise specified, the embodiments and features described in these embodiments can be combined with each other.
[0025] Many specific details are set forth in the following description in order to provide a full understanding of this application. However, this application may also be implemented in other ways different from those described herein. Therefore, the scope of protection of this application is not limited to the specific embodiments disclosed below.
[0026] The following reference Figures 1 to 4 This application describes a continuous flow microchannel reactor for the synthesis of ruthenium complexes according to some embodiments.
[0027] Please see Figures 1 to 4 This application provides a continuous flow microchannel reactor for the synthesis of ruthenium complexes, comprising: a three-necked flask 1; a micro-network channel tube 2, arranged in a serpentine shape within the three-necked flask 1, with its inner wall coated with a corrosion-resistant material layer; a first neck tube 3, connected to the upper left end of the three-necked flask 1; and a microchannel feed assembly 6, consisting of a feed tube and a flow controller, located at the inlet of the first neck tube 3, for connecting and inputting ruthenium, ligands, solvents, and inert gases. The inlet of the first neck tube 3 is covered with a first sealing plug 3. The outlet of the microchannel feed assembly 6 is connected to a microchannel feed tube 7, which extends through the first sealing plug 3 into the first neck tube 3 and the three-necked flask 1. The head end of the micro-network channel tube 2 is connected to the end end of the microchannel feed tube 7.
[0028] In this embodiment, a microchannel feed assembly 6, consisting of a feed tube and a flow controller, is used to connect and input ruthenium, ligands, solvent, and inert gas. The flow controller regulates the feed flow rate from 0.1 to 10 mL / min to maintain the oxygen content of the reaction system below 10 ppm, thereby ensuring normal reaction conditions. Ruthenium, ligands, solvent, and inert gas enter the micro-network channel tube 2. Under the premise of heating the outer bottle 11 and the three-necked flask 1, ruthenium, ligands, solvent, and inert gas react in the micro-network channel tube 2. Since the micro-network channel tube 2 is set in a serpentine shape, a serpentine static mixing unit is formed, which helps to prolong the residence time of ruthenium, ligands, solvent, and inert gas in the three-necked flask, thereby enhancing the mass transfer efficiency of ruthenium, ligands, solvent, and inert gas.
[0029] In some embodiments, the micronetwork channel tube 2 is arranged in a serpentine shape inside the three-necked bottle 1, and the inner wall is coated with a corrosion-resistant material layer.
[0030] In this embodiment, the corrosion-resistant material layer inside the micro-network channel tube 2 is preferably made of polytetrafluoroethylene (PTFE), and the thickness is set to 10-50 μm. Since PTFE is inert to most chemicals and solvents, it can withstand strong acids and alkalis, water and various organic solvents, including aqua regia and fluoroantimony sulfonic acid, and also has high temperature and low temperature resistance, which helps to ensure the service life of the micro-network channel tube 2.
[0031] In some embodiments, a second neck tube 4 is connected to the middle of the upper end of a three-necked flask 1; a temperature detector 8 and a temperature detection probe 9 are disposed at the opening of the second neck tube 4 for real-time detection of the reaction temperature inside the three-necked flask 1; a second sealing plug 17 is provided at the opening of the second neck tube 4; one end of the temperature detector 8 is connected to the temperature detection probe 9; and the temperature detection probe 9 extends through the second sealing plug 17 into the first neck tube 3 and the three-necked flask 1.
[0032] In this embodiment, the temperature inside the three-necked flask 1 is monitored by the cooperation of the temperature detector 8 and the temperature detection probe 9. The temperature is monitored in real time by the sensor data, which is conducive to the real-time detection of the reaction temperature inside the three-necked flask and the real-time adjustment of the reaction conditions, thereby ensuring that the temperature is between 20-150°C to prevent temperature runaway and effectively ensure the quality of the ruthenium complex.
[0033] In some embodiments, the outer bottle 11 is fitted over the three-necked bottle 1, and a media flow channel is provided between the three-necked bottle 1 and the outer bottle 11. The outer bottle 11 has an inlet 14 on one side and an outlet 15 on the other side.
[0034] In this embodiment, a constant-temperature hot melt medium or cooling medium is injected into the media flow channel between the outer bottle 11 and the three-necked bottle 1 through the feed port 14, which is beneficial for the medium in the micro-network channel tube 2 to undergo a constant-temperature high or low temperature reaction, while the discharge port 15 is used to discharge the used hot melt medium or cooling medium.
[0035] In some embodiments, a third neck tube 5 is connected to the upper right end of a three-necked bottle 1; a third sealing plug 18 is provided at the opening of the third neck tube 5; a microchannel outlet tube 10 is provided inside the third neck tube 5; one end of the microchannel outlet tube 10 is connected to the end of a micronetwork channel tube 2; and the microchannel outlet tube 10 extends out of the third neck tube 5 through the third sealing plug 18; the other end of the microchannel outlet tube 10 is connected to a serpentine cooling tube 19; the lower end of the serpentine cooling tube 19 is connected to a reaction processor 12; and the lower end of the reaction processor 12 is connected to a microprocessor 13.
[0036] In this embodiment, after the ruthenium complex in the micro-network channel tube 2 has completed its reaction, it is discharged through the micro-channel outlet tube 10 and then cooled through the serpentine cooling tube 19. After cooling, it is sequentially discharged into the reaction processor 12 and the microprocessor 13 to continue the subsequent reaction (here, the specific reaction process is the prior art, so this technical solution will not be described in detail).
[0037] In some embodiments, the three-necked bottle 1 is made of borosilicate glass.
[0038] In this embodiment, the three-necked bottle 1 made of high borosilicate glass has low expansion rate, high temperature resistance, high strength, high hardness, high light transmittance and high chemical stability, thereby effectively ensuring the durability of the three-necked bottle 1.
[0039] In this application, it should be noted that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "axial," "radial," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this application 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 application.
[0040] 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 at least one of that feature. In the description of this application, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified.
[0041] In this application, unless otherwise expressly specified and limited, the terms "installation" and "connection" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; 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. The term "multiple" refers to two or more, unless otherwise expressly limited. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.
[0042] In this application, unless otherwise expressly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.
[0043] In this application, the terms "one embodiment," "some embodiments," "specific embodiment," etc., refer to a specific feature, structure, material, or characteristic described in connection with that embodiment or example, which is included in at least one embodiment or example of this application. 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.
[0044] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.
Claims
1. A continuous flow microchannel reactor for the synthesis of ruthenium complexes, characterized in that, The utility model relates to a kind of media flow channel reaction device, including: Three-necked bottle (1); Micro-network channel pipe (2), it is in three-necked bottle (1) in serpentine, and inner wall is coated with corrosion-resistant material layer; First neck pipe (3), it is communicated in the upper left end of three-necked bottle (1); Micro-channel feeding assembly (6) is by feeding pipe and flow controller, it is located in the pipe orifice of first neck pipe (3), for connecting input ruthenium, ligand, solvent and inert gas; Second neck pipe (4), it is communicated in the upper middle of three-necked bottle (1); Temperature detector (8) and temperature detection probe (9), it is located in the pipe orifice of second neck pipe (4), for real-time detection reaction temperature in three-necked bottle (1); Third neck pipe (5), it is communicated in the upper right end of three-necked bottle (1); Outer bottle (11), it is set in three-necked bottle (1) outside, and three-necked bottle (1) and outer bottle (11) between leaving media flow channel.
2. A continuous flow microreactor for the synthesis of ruthenium complexes according to claim 1, characterized in that, The pipe orifice of first neck pipe (3) is covered with first sealing plug (16), the discharge port of micro-channel feeding assembly (6) is communicated with micro-channel feeding pipe (7), and micro-channel feeding pipe (7) extends into first neck pipe (3) and three-necked bottle (1) by first sealing plug (16), the first end of micro-network channel pipe (2) is communicated with the end of micro-channel feeding pipe (7).
3. A continuous flow microchannel reactor for the synthesis of ruthenium complexes according to claim 1, characterized in that, The pipe orifice of second neck pipe (4) is covered with second sealing plug (17), one end of temperature detector (8) is connected with temperature detection probe (9), and temperature detection probe (9) extends into first neck pipe (3) and three-necked bottle (1) by second sealing plug (17).
4. The continuous flow microchannel reactor for synthesis of ruthenium complexes according to claim 1, wherein, The pipe orifice of third neck pipe (5) is covered with third sealing plug (18), and micro-channel outlet pipe (10) is arranged in third neck pipe (5), one end of micro-channel outlet pipe (10) is communicated with the end of micro-network channel pipe (2), and micro-channel outlet pipe (10) extends out of third neck pipe (5) by third sealing plug (18).
5. The continuous flow microchannel reactor for synthesis of ruthenium complexes according to claim 1, wherein, The side of outer bottle (11) is provided with feeding port (14), and the other side of outer bottle (11) is provided with discharge port (15).
6. The continuous flow microchannel reactor for synthesis of ruthenium complexes according to claim 1, wherein, Three-necked bottle (1) is made of high borosilicate glass.
7. A continuous flow microreactor for the synthesis of ruthenium complexes according to claim 4, characterized in that, The other end of micro-channel outlet pipe (10) is communicated with serpentine cooling pipe (19), the lower end of serpentine cooling pipe (19) is communicated with reaction processor (12), and the lower end of reaction processor (12) is communicated with microprocessor (13).