Coil reactor and system for flow chemistry

Abstract

The utility model discloses a coil reactor and a system for flow chemistry. The coil reactor comprises a heat conduction inner core, a reaction coil and a shell, the heat-conducting inner core is made of a heat-conducting material, is internally provided with a heating rod and is fixed by heat-conducting glue; the heating rod is provided with an external wire or interface for connecting a power supply and a temperature control device; the reaction coil is of a spiral coil structure and is wound on the outer surface of the heat-conducting inner core, and joints at two ends of the reaction coil are used for connecting external liquid, namely a fluid inlet and a fluid outlet; the shell is matched with the heat-conducting inner core, the reaction coil pipe is clamped between the shell and the heat-conducting inner core, the heat-conducting inner core, the reaction coil pipe and the shell are tightly attached, and if a gap exists between the reaction coil pipe and the heat-conducting inner core and / or the shell, the gap is filled with a heat-conducting medium. The coil reactor disclosed by the utility model is rapid, accurate and uniform in temperature control, small and flexible in structure, convenient to mount, replace and dismount, and convenient to use; and fluid heat transfer is not used, so that leakage risk is avoided, and safety and convenience are achieved.

Description

Technical Field

[0001] This application relates to the field of flow chemical reaction apparatus technology, and in particular to a coil reactor and system for flow chemistry. Background Technology

[0002] Flow chemistry, also known as continuous flow chemistry, is a method of conducting chemical reactions in a continuously flowing fluid. The general process involves one or more reactants being pumped into a mixing device and then flowing through a flow chemistry reactor under controlled reaction conditions (temperature, light, etc.) until the reaction is complete, while the reaction mixture is continuously collected at the reactor outlet. Compared to traditional indirect chemistry, flow chemistry offers advantages such as high mass and heat transfer efficiency, high reaction safety, precise material proportioning, good production reproducibility, and high automation. Therefore, flow chemistry is receiving increasing attention and is being used in synthetic applications.

[0003] Flow chemical reactors, also known as microchannel reactors, are the core unit of flow chemistry technology and are crucial in determining the quality of flow chemical processes. Flow chemical reactors are reactors composed of millimeter or sub-millimeter level channels, offering advantages such as large specific surface area, high mixing efficiency, excellent heat and mass transfer, narrow residence time distribution, and safety. Flow chemical reactors have broad application prospects in chemical synthesis, chemical kinetics research, and process development; they are increasingly used in research on reactions that are difficult to control under conventional conditions, such as strongly exothermic rapid reactions, catalytic oxidation of hydrocarbons, and organometallic catalytic coupling. Common flow chemical reactors include coil reactors, chip reactors, and packed bed reactors.

[0004] Coil reactors are typically composed of plastic or metal tubes wound into a disc shape, combined with devices for controlling reaction conditions such as temperature and light. Due to their low cost and simple manufacturing process, coil reactors are the most widely used reactors in flow chemistry.

[0005] Temperature control is a common requirement in flow chemistry. Currently, most coil reactors are immersed in a water bath or oil bath, and the reactor temperature is controlled by adjusting the temperature of the water bath or oil bath. However, this method of temperature control has the following disadvantages: 1. Slow rate of temperature change in the water bath or oil bath; 2. Large size and inconvenient use of the device used to control the temperature of the water bath or oil bath; 3. Prone to overflow or leakage of the water bath or oil bath; 4. Inconvenient operation during installation or replacement.

[0006] Therefore, how to achieve more efficient, accurate, simple, and convenient temperature control of coil reactors remains a critical technical challenge that needs to be addressed in the field of flow chemistry. Summary of the Invention

[0007] The purpose of this application is to provide an improved coil reactor for flow chemistry, and a flow chemistry reaction system based on the coil reactor.

[0008] To achieve the above objectives, this application adopts the following technical solution:

[0009] One aspect of this application discloses a coil reactor for flow chemistry, comprising a thermally conductive inner core, a reaction coil, and a shell. The thermally conductive inner core is made of a thermally conductive material, and a heating rod is installed inside the thermally conductive inner core and fixed with thermally conductive adhesive. The heating rod has an external wire or external interface for connecting a power supply and a temperature control device. The reaction coil has a helical coil structure and is wound around the outer surface of the thermally conductive inner core. The connectors at both ends of the reaction coil are used to connect to an external liquid transfer system, serving as the inlet and outlet of the reaction liquid fluid of the reaction coil, respectively. The shell cooperates with the thermally conductive inner core, clamping the reaction coil between the shell and the thermally conductive inner core, and the three are tightly fitted together. If there is a gap between the reaction coil and the thermally conductive inner core and / or the shell, it is filled with a thermally conductive medium.

[0010] The thermally conductive materials used in this application include, but are not limited to, thermally conductive metals or thermally conductive ceramics. The reaction conduits in this application are generally hollow metal conduits, such as stainless steel hollow conduits. The reaction coil can be formed by directly winding the reaction conduit around the outer surface of the thermally conductive inner core, or it can be prefabricated as a coil structure for direct assembly during use. Specific implementations of the outer shell include, for example, the outer shell directly wrapping around the reaction coil, or the outer shell being mounted on the thermally conductive inner core, with the two forming a cavity to accommodate the reaction coil.

[0011] It should be noted that the coil reactor of this application achieves rapid temperature control through electric heating and by using an outer shell and a heat-conducting medium to fill the gaps, resulting in accurate and uniform temperature control. The coil reactor of this application has a compact and flexible structure, is easy to use, does not use fluid heat transfer, eliminates the risk of leakage, and is therefore safer and more convenient. In one implementation of this application, the outer shell adopts a quick-connect structure, making installation, replacement, and disassembly convenient and easy to use.

[0012] In one implementation of this application, the coil reactor further includes a temperature sensor for real-time monitoring of the temperature of the coil reactor; the temperature sensor has an external wire or an external interface for connecting to a temperature control device.

[0013] In one implementation of this application, the temperature sensor is installed inside the thermally conductive inner core and fixed with thermally conductive adhesive.

[0014] It should be noted that the distance between the temperature sensor and the heating rod in this application is greater than or equal to 5 mm, so as to more effectively reflect the true temperature of the reaction coil. It is understood that if the temperature sensor is too close to the heating rod, it will be too affected by the temperature of the heating rod and will not be able to reflect the true temperature of the reaction coil.

[0015] In one implementation of this application, the coil reactor further includes a base, and a heat-conducting inner core and / or outer shell are detachably and fixedly mounted on the base.

[0016] In one implementation of this application, both the thermally conductive adhesive and the thermally conductive medium are thermally conductive silicone.

[0017] In one implementation of this application, the gap between the reaction pipes wound in the reaction coil is less than or equal to 1.0 mm.

[0018] It should be noted that the gap between the wound reaction pipes should theoretically be as small as possible. This application study believes that as long as the gap is less than or equal to 1.0 mm and is filled with a heat-conducting medium, the gap has little impact on the accuracy, stability and uniformity of heating, and can meet the application requirements of this application.

[0019] In one implementation of this application, the gap between the reaction coil and the heat-conducting inner core is 0-0.5 mm; the gap between the reaction coil and the outer shell is 0-0.5 mm.

[0020] It should be noted that, theoretically, the smaller the gap between the reaction coil and the heat-conducting inner core or outer shell, the better; however, considering the processing progress and assembly errors, gaps are inevitable. This application study believes that when the gap is 0-0.5mm and there is a heat-conducting medium filling it, the gap has little impact on the accuracy, stability and uniformity of heating, and can meet the application requirements of this application.

[0021] In one implementation of this application, the distance between the heating rod and the reaction coil is greater than or equal to 5 mm.

[0022] In one implementation of this application, the outer shell is made of a thermally conductive material or a thermally insulating material.

[0023] It should be noted that in this application, when both the heat-conducting inner core and the outer shell are made of a material with high thermal conductivity, one specific implementation uses the same material. The heat-conducting inner core and the outer shell are in close contact with the reaction coil. Furthermore, in areas where the reaction coil is not placed, the heat-conducting inner core and the outer shell are also in close contact, directly in contact, or filled with a heat-conducting medium. This allows heat transfer to quickly reach the same temperature, forming a constant-temperature cavity in the middle, which is the location where the coil is placed. This design, on the one hand, places the reaction coil in a constant-temperature cavity, making it easy to maintain a constant temperature; on the other hand, the close contact between the coil and the heat-conducting inner core and the outer shell ensures fast heat transfer and sensitive and accurate temperature control. In use, an additional insulation layer can be selectively wrapped around the outer shell for better insulation; since the reaction coil is in the sandwich between the heat-conducting inner core and the outer shell, an insulation layer is not necessary. When the outer shell is made of a heat-insulating material, the heat-conducting inner core is heated, and the outer shell is insulated, forming a constant-temperature cavity between the heat-conducting inner core and the outer shell, eliminating the need for an additional insulation layer.

[0024] Another aspect of this application discloses a flow chemical reaction system that uses the coil reactor of this application as the flow chemical reactor.

[0025] It should be noted that the key to the fluid chemical reaction system of this application is the use of the coil reactor of this application. As for other structures of the system, such as reagent storage, switching valve, pump, preheater, control system, etc., they can refer to the prior art. The connection method of each component can also refer to the prior art, and no specific limitation is made here.

[0026] Due to the adoption of the above technical solutions, the beneficial effects of this application are as follows:

[0027] The coil reactor of this application has the advantages of rapid, accurate and uniform temperature control; moreover, it has a compact and flexible structure, is easy to use, and is convenient to install, replace and disassemble; more importantly, the coil reactor of this application does not use fluid heat transfer, has no risk of leakage, and is safer and more convenient. Attached Figure Description

[0028] Figure 1 This is an exploded structural diagram of the coil reactor in an embodiment of this application;

[0029] Figure 2 This is a schematic diagram of the assembly structure of the coil reactor in the embodiments of this application;

[0030] Figure 3 This is a schematic diagram of the structure of the reaction coil in the embodiments of this application;

[0031] Figure 4 This is a temperature rise curve of the coil reactor in the embodiments of this application;

[0032] Figure 5This is a temperature control curve of the coil reactor in the embodiments of this application. Detailed Implementation

[0033] To achieve simpler, more accurate, and more uniform temperature control, and to reduce the size of the reactor, this application develops an improved coil reactor for flow chemistry.

[0034] Specifically, the coil reactor of this application includes: a thermally conductive inner core, a reaction coil, and an outer shell; the thermally conductive inner core is made of a thermally conductive material, and a heating rod is installed inside the thermally conductive inner core and fixed with thermally conductive adhesive; the heating rod has an external wire or external interface for connecting a power supply and a temperature control device; the reaction coil is formed by winding a reaction pipe around the outer surface of the thermally conductive inner core, and the joints at both ends of the reaction coil are used to connect to an external liquid transfer system, serving as the reaction liquid inlet and outlet of the reaction coil, respectively; the outer shell is wrapped around the reaction coil, and the thermally conductive inner core, the reaction coil, and the outer shell are tightly fitted together. If there is a gap between the reaction coil and the thermally conductive inner core and / or the outer shell, it is filled with a thermally conductive medium.

[0035] The coil reactor of this application has the following advantages compared with existing flow chemical reactors:

[0036] 1. It adopts electric heating, a jacketed structure and heat-conducting medium to fill the gaps, which can achieve rapid heating. It only takes 3 minutes for the temperature to change by 10℃, and the temperature control is accurate and uniform.

[0037] 2. In one implementation of this application, a stainless steel coil and an aluminum alloy or copper jacket structure are used, which is compact, flexible and easy to use.

[0038] 3. No liquid medium heat bath is used, so there is no risk of leakage.

[0039] 4. The quick-connect jacket structure makes installation, replacement, and disassembly convenient and easy to use.

[0040] The following is an explanation of some of the key technical terms involved in this application:

[0041] Flow chemistry, also known as continuous flow chemistry, is a method of conducting chemical reactions in a continuously flowing fluid. The general process involves one or more reactants being pumped into a mixing device, then flowing through a flow chemistry reactor where reaction conditions, such as temperature and illumination, are controlled until the reaction is complete. Simultaneously, the reaction mixture is continuously collected at the reactor outlet. Compared to traditional indirect chemistry, flow chemistry offers advantages such as high mass and heat transfer efficiency, high reaction safety, precise material proportioning, good production reproducibility, and a high degree of automation.

[0042] Flow chemical reactors, also known as microchannel reactors, are reactors composed of millimeter or sub-millimeter level channels. They offer advantages such as large specific surface area, excellent heat and mass transfer, and safety. Common types of flow chemical reactors include coil reactors, wafer reactors, and packed bed reactors.

[0043] The present application will now be described in further detail with reference to specific embodiments and accompanying drawings. In the following embodiments, many details are described to facilitate a better understanding of the present application. However, those skilled in the art will readily recognize that some features may be omitted in different situations, or may be replaced by other devices, materials, or methods. In some cases, certain operations related to the present application are not shown or described in the specification to avoid obscuring the core parts of the application with excessive description. For those skilled in the art, detailed description of these related operations is not necessary; a complete understanding of the related operations can be obtained from the description in the specification and general technical knowledge in the art.

[0044] Example

[0045] This example uses a coil reactor for flow chemistry, such as... Figure 1 and Figure 2 As shown, the device includes a thermally conductive inner core 1, a reaction coil 2, and a shell 3. The thermally conductive inner core is made of thermally conductive metal or ceramic; in this example, it is made of aluminum alloy with an outer diameter of 40mm, a hollow cavity diameter of 16mm, and a total length of 85mm. Copper is also a good choice, as it has good thermal conductivity, high strength, and is not easily deformed. An electric heating rod 11, 6mm in diameter and 40mm in length, is installed inside the thermally conductive inner core and fixed with thermally conductive silicone grease. The heating rod 11 has an external wire or interface for connecting to a power supply and temperature control device; in this example, an external interface is used. The reaction coil 2 is formed by winding a reaction pipe around the outer surface of the thermally conductive inner core, as shown... Figure 2 As shown, the connectors at both ends of the reaction coil are used to connect to an external liquid transfer system, serving as the inlet and outlet of the reaction liquid fluid, respectively. In this example, inlet connector 21 and outlet connector 22 are designed at both ends of the reaction coil for connecting to the liquid transfer system. The reaction pipe in this example is made of stainless steel, with an outer diameter of 1.6 mm and an inner diameter of 1 mm, wound to form a reaction coil with an inner diameter of 40 mm and a length of 50 mm. The outer shell 3 wraps around the reaction coil 2, and the heat-conducting inner core 1, the reaction coil 2, and the outer shell 3 are tightly fitted together, with a heat-conducting medium filling the gap between the reaction coil 2 and the outer shell 3. The outer shell is made of aluminum alloy, with an outer diameter of 51 mm, an inner diameter of 43.2 mm, and a length of 85 mm; the filling heat-conducting medium is thermal grease.

[0046] In a further improvement to this example, the coil reactor also includes a temperature sensor 12, 5mm in diameter and 20mm in length, with an M6 external thread at the bottom. It is threaded onto the inner core, and the gap between the temperature sensor and the inner core is filled with thermally conductive silicone grease for real-time monitoring of the coil reactor's temperature. The temperature sensor has an external interface for connecting a temperature control device. In this example, the temperature sensor 12 is installed inside the thermally conductive inner core 1 and fixed with thermally conductive adhesive. Furthermore, the coil reactor in this example also includes a base 4. The thermally conductive inner core 1 and the outer shell 3 are detachably and fixedly mounted on the base 4. In this example, the base is made of corrosion-resistant Teflon material and requires thermal insulation; its dimensions are 80*80*30mm.

[0047] In this example of a coil reactor, there are no gaps between the wound coils, such as... Figure 3 As shown; it's understandable that gaps will affect heat transfer to varying degrees. In principle, gaps less than 1.0mm have minimal impact, though the heat transfer effect will be slightly worse. The optimal gap between the coil and the jacket is 0-0.5mm. Too small a gap makes coil installation difficult, while too large a gap affects heat transfer; in this example, it's 0.1mm. The gap between the coil and the heat-conducting inner core is also 0-0.5mm, ideally smaller. Considering manufacturing and installation errors, a gap less than 0.5mm, and with a heat-conducting medium filling it, has minimal impact on heat transfer. The heating rod is approximately 5cm long; length is not critical. The heating rod is specifically mounted on the cylindrical structure inside the jacket. The distance between the heating rod and the coil should ideally be greater than or equal to 5mm for more uniform temperature control; in this example, it's 5mm.

[0048] Temperature control experiments were conducted on the coil reactor prepared in this example to test its heating rate, isothermal stability, and heating uniformity. The specific testing methods are as follows:

[0049] 1. Heating rate test

[0050] The coil reactor in this example was connected to a solid-state relay-type temperature controller and a power supply. At a room temperature of approximately 25°C, the heating rod was set to temperatures of 60°C, 80°C, 100°C, and 120°C. The temperature rise curves of the coil reactor at different heating temperatures were statistically analyzed. In this example, an infrared thermometer was used to measure the surface temperature of the coil. The results are as follows: Figure 4 As shown.

[0051] Figure 4The results show that when the temperature is set to 60℃, it takes approximately 8 minutes to reach 60℃ and then stabilizes at the set temperature. Similarly, when the temperature is set to 80℃, 100℃, and 120℃, the times to reach the set temperature are 14 minutes, 18 minutes, and 30 minutes, respectively. Furthermore, it can be observed that the heating curve includes a linear region and a plateau region. The linear region overlaps when different temperatures are set, with a heating rate of approximately 10℃ every 2.5 minutes, indicating that the coil reactor in this example can achieve rapid heating. Approaching the set temperature, it enters a plateau region, reaching the set value smoothly and accurately without significant deviation. Therefore, the coil reactor in this example can achieve rapid heating and precise temperature control.

[0052] 2. Constant Temperature Stability Test

[0053] The connection method is the same as in "1. Heating Rate Test". At a room temperature of approximately 25°C, the reactor temperature was set to 60°C. The test began after the temperature reached 60°C and stabilized for 5 minutes. An infrared thermometer was used to measure the surface temperature of the coil, recording the temperature every 10 seconds for a total of 420 seconds. The results are as follows: Figure 5 As shown.

[0054] Figure 5 The results showed that when the temperature was set to 60℃, the reactor temperature varied between 59.6℃ and 60.4℃, with a temperature control error of ±0.4℃. This indicates that the temperature control of the coil reactor in this example is accurate and has good stability.

[0055] 3. Heating uniformity test

[0056] The connection method is the same as "1. Heating rate test". Under the condition of room temperature of about 25°C, the reactor temperature is set to 60°C. The test begins after the temperature reaches 60°C and stabilizes for 5 minutes. On the coil (i.e., reaction coil) of the reactor, five measurement points are taken at equal intervals from the inlet to the outlet of the reaction liquid. The five measurement points evenly cover the entire coil. The surface temperature of the coil is measured with an infrared thermometer. The temperature of the measurement point is recorded every 60 seconds for a total of 360 seconds. The results are shown in Table 1.

[0057] Table 1 Temperature measurement results at different locations on the reaction coil

[0058] Second 0 60 seconds 120 seconds 180 seconds 240 seconds 300 seconds 360 seconds Measurement point 1 60.1℃ 60.3℃ 60.2℃ 60.4℃ 60.2℃ 60.1℃ 60.0℃ Measurement point 2 59.8℃ 59.7℃ 59.9℃ 59.9℃ 59.6℃ 59.8℃ 59.7℃ Measurement point 3 60.3℃ 60.5℃ 60.4℃ 60.3℃ 60.2℃ 60.3℃ 60.4℃ Measurement point 4 60.5℃ 60.4℃ 60.6℃ 60.2℃ 60.7℃ 60.5℃ 60.4℃ Measurement point 5 59.6℃ 59.3℃ 59.5℃ 59.7℃ 59.8℃ 59.7℃ 59.5℃

[0059] Table 1 shows that when the temperature is set to 60℃, the temperature variation at the same measurement point is within 0.5℃, indicating accurate temperature control and small temperature fluctuations. The temperatures at the five temperature measurement points in the reactor ranged from a high of 59.3℃ to a low of 60.7℃, with a temperature control error of ±0.7℃. The maximum temperature difference at different locations was within 1.4℃, indicating that the reactor temperature control is very uniform and the temperature differences between different locations are small.

[0060] The coil reactor in this example achieves rapid and uniform temperature control through electric heating, a jacketed insulation cavity, and a heat-conducting medium filling the gaps. The temperature control is accurate and uniform. This example uses a stainless steel coil and a metal jacket structure, which is compact, flexible, and easy to use. Installation, replacement, and disassembly are convenient. In addition, it does not use fluid heat transfer, eliminating the risk of leakage and making it safer and more convenient.

[0061] The above description, in conjunction with specific embodiments, provides a further detailed explanation of this application and should not be construed as limiting the specific implementation of this application to these descriptions. Those skilled in the art to which this application pertains can make several simple deductions or substitutions without departing from the concept of this application.

Claims

1. A coil reactor for flow chemistry, characterized by: It includes a thermally conductive inner core (1), a reaction coil (2), and an outer shell (3); The thermally conductive inner core is made of thermally conductive material, and a heating rod (11) is installed inside the thermally conductive inner core and fixed with thermally conductive adhesive; The heating rod (11) has an external wire or an external interface for connecting a power supply and a temperature control device; The reaction coil (2) has a spiral coil structure and is wound around the outer surface of the heat-conducting inner core (1). The connectors at both ends of the reaction coil are used to connect to an external liquid transmission system, which serve as the reaction liquid inlet and outlet of the reaction coil, respectively. The outer shell (3) cooperates with the heat-conducting inner core (1) to sandwich the reaction coil (2) between the outer shell (3) and the heat-conducting inner core (1), and the heat-conducting inner core (1), the reaction coil (2) and the outer shell (3) are tightly fitted together. If there is a gap between the reaction coil (2) and the heat-conducting inner core (1) and / or the outer shell (3), a heat-conducting medium is used to fill it.

2. The coil reactor of claim 1, wherein: It also includes a temperature sensor (12) for real-time monitoring of the temperature of the coil reactor; the temperature sensor has an external wire or external interface for connecting to a temperature control device.

3. The coil reactor of claim 2, wherein: The temperature sensor (12) is installed inside the thermally conductive inner core (1) and fixed with thermally conductive adhesive.

4. The coil reactor of claim 1, wherein: It also includes a base (4), a thermally conductive inner core (1) and / or a housing (3) which are detachably fixedly mounted on the base (4).

5. The coil reactor according to any one of claims 1 to 4, characterized in that: Both the thermally conductive adhesive and the thermally conductive medium are thermally conductive silicone.

6. The coil reactor according to any one of claims 1 to 4, characterized in that: In the reaction coil (2), the gap between the wound reaction pipes is less than or equal to 1.0 mm.

7. The coil reactor according to any one of claims 1 to 4, characterized in that: The gap between the reaction coil (2) and the heat-conducting inner core (1) is 0-0.5 mm; the gap between the reaction coil (2) and the outer shell (3) is 0-0.5 mm.

8. The coil reactor according to any one of claims 1 to 4, characterized in that: The distance between the heating rod (11) and the reaction coil (2) is greater than or equal to 5 mm.

9. The coil reactor according to any one of claims 1 to 4, characterized in that: The outer shell (3) is made of thermally conductive or thermally insulating materials.

10. A flow chemistry reaction system characterized by: This includes using the coil reactor described in any one of claims 1-9 as a flow chemical reactor.

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