A cryogenic reaction apparatus

Abstract

The application discloses a low-temperature reaction device, and relates to the field of chemical experiment equipment, which comprises a support, a mounting seat, a semiconductor refrigeration sheet and a reaction container, the mounting seat is fixedly installed on the support, a plurality of limiting blocks are fixedly installed on the top of the mounting seat, the plurality of limiting blocks are distributed at intervals along the outer contour of the semiconductor refrigeration sheet and are fixedly installed on the mounting seat; a low-temperature cylinder is arranged above the mounting seat, the reaction container is installed in the low-temperature cylinder, the bottom surface of the low-temperature cylinder is attached to the semiconductor refrigeration sheet and is fixedly installed on the mounting seat; a temperature sensor is also fixedly installed on the bottom surface of the low-temperature cylinder, the temperature sensor monitors the reaction environment temperature in real time, and the risk of over-temperature or low-temperature is avoided. The application has the effects of compact structure, high-precision and high-efficiency temperature control, sealing and moisture-proof, energy saving and stability, and convenience in realizing parallel reaction.

Description

Technical Field

[0001] This application relates to the technical field of chemical experimental equipment, and in particular to a low-temperature reaction apparatus. Background Technology

[0002] Low-temperature reaction conditions play a crucial role in organic synthesis, drug development, and fine chemicals. Many organic reactions (such as nucleophilic substitution, electrophilic addition, organometallic reactions, and free radical reactions) often suffer from poor selectivity or are accompanied by side reactions at room temperature. However, at low temperatures, reaction rates can be effectively controlled, side reactions are reduced, intermediate stability is improved, and the yield and selectivity of the target product are significantly enhanced.

[0003] Currently, the commonly used low-temperature control methods in laboratories mainly include two categories: traditional cold bath methods and compressor refrigeration cycles. Traditional cold bath methods (such as ice-water baths, salt-ice baths, dry ice / acetone baths, or liquid nitrogen baths) are simple to operate and have low costs, but they have problems such as unstable temperature, difficulty in maintaining constant temperature for a long time, and insufficient adjustment precision. On the other hand, compressor refrigeration cycles can provide a relatively stable low-temperature environment, but they have limitations such as large system size, complex maintenance, high energy consumption, and difficulty in achieving independent temperature control under the condition of multiple reaction systems in parallel, which restricts their application in efficient synthesis and condition screening. Utility Model Content

[0004] In view of the above-mentioned prior art, in order to solve the problems of unstable temperature, low temperature control accuracy and large volume and high energy consumption of compressor refrigeration cycle in traditional cold bath method, this application provides a low temperature reaction device.

[0005] This application provides a low-temperature reaction apparatus, which adopts the following technical solution: A low-temperature reaction apparatus includes a support, a mounting base, a thermoelectric cooler, and a reaction vessel. The mounting base is fixedly mounted on the support, the thermoelectric cooler is fixedly mounted on the top surface of the mounting base, and the reaction vessel is located above the thermoelectric cooler, with its bottom surface in contact with the thermoelectric cooler. By adopting the above technical solution, the semiconductor cooling chip is directly attached to the bottom surface of the reaction vessel, which can quickly and accurately control the reaction temperature, avoiding the temperature fluctuations of the traditional cold bath method and the bulky problems of the compressor refrigeration cycle, achieving efficient and energy-saving low-temperature reaction. At the same time, the structure is compact and facilitates independent temperature control of parallel reaction systems.

[0006] Preferably, a low-temperature cylinder is provided on the top of the mounting base, the low-temperature cylinder is fixedly mounted on the mounting base, the bottom surface of the low-temperature cylinder is in contact with the semiconductor cooling chip, and the reaction vessel is installed inside the low-temperature cylinder.

[0007] By adopting the above technical solution, the low-temperature cylinder serves as an intermediate heat transfer medium, ensuring that the cooling energy of the semiconductor refrigeration chip is uniformly transferred to the reaction vessel, improving temperature uniformity and cooling efficiency, while protecting the reaction vessel from external interference.

[0008] Preferably, the low-temperature cylinder is provided with a low-temperature protective shell, one end of which is provided with a sealing ring. The low-temperature protective shell is fitted onto the outer periphery of the low-temperature cylinder, the sealing ring is located above the low-temperature cylinder, the inner wall of the sealing ring abuts against the outer periphery of the reaction vessel, and a sealing ring is provided between the sealing ring and the top of the low-temperature cylinder.

[0009] By adopting the above technical solution, the cryogenic protective shell and the sealing ring form a double sealing barrier, effectively preventing external air and moisture from entering the cryogenic cylinder, avoiding condensation or frost, and maintaining the stability and repeatability of reaction conditions.

[0010] Preferably, the cryogenic cylinder is provided with a heat insulation layer around its outer peripheral wall, and the heat insulation layer is located between the cryogenic cylinder and the cryogenic protective shell.

[0011] By adopting the above technical solutions, the insulation layer reduces heat exchange between the low-temperature cylinder and the external environment, improves refrigeration efficiency, reduces energy loss, and prevents surface condensation caused by local overcooling.

[0012] Preferably, the bottom surface of the cryogenic cylinder is provided with an installation groove, and the semiconductor cooling chip is embedded in the installation groove; both sides of the bottom surface of the cryogenic cylinder along the length direction of the installation groove are provided with clearance grooves, and the depth of the clearance grooves is greater than that of the installation groove.

[0013] By adopting the above technical solution, the clearance groove provides crucial operating space for the installation, debugging, and maintenance of the thermoelectric cooler, allowing for non-destructive disassembly and fine-tuning of its position, ensuring tight and flat contact between the thermoelectric cooler and the bottom surface of the cryogenic cylinder. Simultaneously, this structure effectively reduces reverse heat conduction from the heat dissipation end of the thermoelectric cooler to the cooling area by increasing the heat conduction path, lowering the risk of thermal short circuits and thus improving cooling efficiency and temperature control stability.

[0014] Preferably, the bottom surface of the low-temperature cylinder is further provided with a fixing groove, and a temperature sensor is installed in the fixing groove.

[0015] By adopting the above technical solution, the fixing groove ensures that the temperature measuring end of the temperature sensor is in close and stable contact with the bottom surface of the low-temperature cylinder, eliminating temperature measurement errors caused by looseness or gaps; the fixing groove increases the contact area between the sensor and the low-temperature cylinder, improves heat conduction efficiency, and makes temperature feedback more sensitive.

[0016] Preferably, the heat dissipation component is a water-cooled block, which is installed on the heat dissipation end of the semiconductor cooling chip. The water-cooled block has a flow channel inside and an inlet connector and an outlet connector on the water-cooled block for communicating with both ends of the flow channel.

[0017] By adopting the above technical solution, the water-cooled block efficiently dissipates the heat generated by the semiconductor refrigeration chip through circulating coolant, ensuring the semiconductor refrigeration chip operates continuously and stably, maintaining its cooling performance, and extending the service life of the device.

[0018] Preferably, a magnetic stir bar is placed inside the reaction vessel, a rotary motor is provided below the mounting base, the rotary motor is fixedly mounted on the bracket, the output end of the rotary motor faces upward, a mounting plate is provided at the output end of the rotary motor, and magnet blocks are fixedly mounted at both ends of the top surface of the mounting plate along the length direction.

[0019] By adopting the above technical solution, the rotating magnetic field is generated by driving the magnetic block to rotate through the rotating motor. This enables the magnetic stir bar in the reaction vessel to rotate synchronously without contact, thereby achieving uniform and continuous stirring of the reaction materials. The magnetic drive method has a compact structure and good sealing performance. It can achieve the stirring function without penetrating the reaction vessel, making it particularly suitable for use in low-temperature reaction conditions that are closed or require strict isolation from the external environment.

[0020] In summary, this application includes at least one of the following beneficial technical effects: 1. The semiconductor cooling chip is directly attached to the bottom surface of the reaction vessel, which can quickly and accurately control the reaction temperature, avoiding the temperature fluctuations of the traditional cold bath method and the bulky problems of the compressor refrigeration cycle, realizing efficient and energy-saving low-temperature reaction. At the same time, the structure is compact and facilitates independent temperature control of parallel reaction systems. 2. The insulation layer reduces heat exchange between the low-temperature cylinder and the external environment, improves refrigeration efficiency, reduces energy loss, and prevents surface condensation caused by localized overcooling; 3. By rotating the motor to drive the magnet block to rotate, a rotating magnetic field is generated, which can drive the magnetic stir bar in the reaction vessel to rotate synchronously without contact, so as to achieve uniform and continuous stirring of the reaction materials. The magnetic drive method has a compact structure and good sealing performance. It can achieve the stirring function without penetrating the reaction vessel, and is particularly suitable for use in low-temperature reaction conditions that are closed or require strict isolation from the external environment. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the overall structure of this utility model; Figure 2 yes Figure 1 Cross-sectional view at point AA; Figure 3 This is an exploded view of the entire utility model; Figure 4 This utility model is an exploded view showing a low-temperature cylinder and a semiconductor refrigeration chip.

[0022] Reference numerals: 1. Bracket; 2. Mounting base; 3. Semiconductor cooling chip; 4. Reaction vessel; 5. Limiting block; 6. Cryogenic cylinder; 61. Mounting groove; 62. Clearance groove; 63. Fixing groove; 7. Cryogenic protective shell; 71. Mounting cavity; 8. Sealing ring; 9. Insulation layer; 10. Heat sink; 101. Water cooling block; 1011. Water inlet connector; 1012. Water outlet connector; 11. Rotating motor; 12. Mounting plate; 13. Magnet block; 14. Sealing ring. Detailed Implementation

[0023] The following is in conjunction with the appendix Figure 1-4 This application will be described in further detail.

[0024] This application discloses a low-temperature reaction apparatus.

[0025] Reference Figure 1 and Figure 2 A low-temperature reaction apparatus includes a support 1, a mounting base 2, a thermoelectric cooler 3, and a reaction vessel 4. The mounting base 2 is fixedly mounted on the support 1. Multiple limiting blocks 5 are fixedly mounted on the top of the mounting base 2. The multiple limiting blocks 5 are spaced apart along the outer contour of the thermoelectric cooler 3 and fixedly mounted on the mounting base 2. Heat dissipation components 10 for dissipating heat from the thermoelectric cooler 3 are provided between the multiple limiting blocks 5. A low-temperature cylinder 6 is fixedly mounted on the mounting base 2. The reaction vessel 4 is installed inside the low-temperature cylinder 6. The thermoelectric cooler 3 is installed on the bottom surface of the low-temperature cylinder 6. A temperature sensor is also fixedly mounted on the bottom surface of the low-temperature cylinder 6. The temperature sensor monitors the reaction environment temperature in real time to avoid the risk of overheating or underheating.

[0026] Reference Figure 3 and Figure 4 The cryogenic cylinder 6 has a mounting groove 61 on its bottom surface. The semiconductor cooling chip 3 is embedded in the mounting groove 61, and the cooling part of the semiconductor is completely wrapped by the inner wall of the mounting groove 61. On both sides of the bottom surface of the cryogenic cylinder 6 along the length of the mounting groove 61, there are clearance grooves 62, the depth of which is greater than the depth of the mounting groove 61. The mounting groove 61 ensures a tight fit between the semiconductor cooling chip 3 and the bottom surface of the cryogenic cylinder 6, increasing the contact area, reducing thermal resistance, and improving cooling efficiency. The operator can observe whether the cooling chip is installed correctly and evenly through the clearance grooves 62, and make fine adjustments to ensure optimal contact with the bottom surface of the cryogenic cylinder 6.

[0027] The bottom surface of the cryogenic cylinder 6 is also provided with a fixing groove 63, in which the temperature sensor is fixedly installed. The fixing groove 63 ensures that the temperature measuring end of the temperature sensor is in close and stable contact with the bottom surface of the cryogenic cylinder, eliminating temperature measurement errors caused by looseness or gaps; the fixing groove 63 increases the contact area between the sensor and the cryogenic cylinder 6, improves heat conduction efficiency, and makes the temperature feedback more sensitive.

[0028] The upper edge of the reaction vessel 4 is higher than the upper edge of the cryogenic cylinder 6. A cryogenic protective shell 7 is arranged around the outer periphery of the cryogenic cylinder 6, and a sealing ring 8 is provided on the top of the cryogenic protective shell 7. When the protective shell is installed in place, the sealing ring 8 is located above the cryogenic cylinder 6, and its inner wall abuts against the outer periphery of the reaction vessel 4 near the upper edge. In addition, a sealing ring 14 is installed between the sealing ring 8 and the top of the cryogenic cylinder 6, and the sealing ring 14 is arranged around the outer periphery of the reaction vessel 4. Through the tight abutment between the sealing ring 8 and the outer wall of the reaction vessel 4, combined with the sealing ring 14 between the sealing ring 8 and the top of the cryogenic cylinder 6, a double sealing barrier is formed, effectively preventing external air and moisture from entering the interior of the cryogenic cylinder 6, and avoiding the influence of external environmental interference on the stability of the reaction conditions.

[0029] Reference Figure 3 The cryogenic protective shell 7 is bent radially outward on one side, forming an installation cavity 71 between the cryogenic protective shell 7 and the cryogenic cylinder 6. An insulation layer 9 is provided around the circumference of the cryogenic cylinder 6, located within the installation cavity 71 between the cryogenic protective shell 7 and the cryogenic cylinder 6. The radial outward bending of the cryogenic protective shell 7 naturally forms the installation cavity 71 with the cryogenic cylinder 6, providing a dedicated and well-organized space for the insulation layer 9, eliminating the need for additional fixing structures and making the overall device more compact. The insulation layer 9 completely covers the outer circumference of the cryogenic cylinder 6, preventing direct contact between the outer wall of the cryogenic cylinder 6 and the outside air, thus avoiding surface condensation or frost due to localized overcooling.

[0030] The heat sink 10 is a water-cooled block 1011. The heat dissipation end of the thermoelectric cooler 3 is connected to the water-cooled block 1011. The water-cooled block 101 is fixedly installed on the top of the mounting base 2. The water-cooled block 101 has the same outline as the thermoelectric cooler 4 and is embedded between multiple limiting blocks 5. A flow channel is opened inside the water-cooled block 101. A water inlet connector 1011 and a water outlet connector 1012, which communicate with both ends of the flow channel, are fixedly installed on the water-cooled block 101. When the thermoelectric cooler 3 is cooled, the coolant flows into the flow channel inside the water-cooled block 101 through the water inlet connector 1011, flows through the bottom of the hot end of the thermoelectric cooler 3 and absorbs the heat generated therefrom, and then is discharged from the water outlet connector 1012, thereby achieving continuous and efficient heat removal and maintaining the cooling performance and working stability of the thermoelectric cooler 3.

[0031] A magnetic stir bar is placed inside the reaction vessel 4. A rotating motor 11 is installed below the mounting base 2. A horizontal mounting plate 12 is fixedly installed at the output end of the rotating motor 11. Magnet blocks 13 are fixedly installed at both ends of the top surface of the mounting plate along the length direction. The magnet blocks 13 and the magnetic stir bar are attracted to each other by opposite poles. The magnetic pole of the magnet blocks 13 is N-pole, and the magnetic pole of the magnetic stir bar is S-pole.

[0032] When the material in the reaction vessel 4 is stirred, the rotating motor 11 is started, driving the mounting plate 12 and the magnetic block 13 on its top surface to rotate. At this time, the magnetic block 13 and the magnetic stir bar in the reaction vessel 4 attract each other through opposite magnetic poles (N pole and S pole). The rotating magnetic field generated by the rotating magnetic block 13 will drive the magnetic stir bar to rotate synchronously, thereby continuously and uniformly stirring the liquid or mixture in the reaction vessel 4.

[0033] The implementation principle of this application embodiment is as follows: The semiconductor cooling chip 3 directly contacts the bottom surface of the reaction vessel 4, providing rapid and precise cooling control, avoiding the temperature fluctuations of traditional cold bath methods and the bulky and energy-intensive problems of compressor refrigeration cycles. The cooling energy of the semiconductor cooling chip 3 is uniformly transferred to the reaction vessel 4 through the cryogenic cylinder 6 as a heat transfer medium, ensuring a consistent temperature distribution in the reaction area and improving cooling efficiency and temperature stability. A temperature sensor monitors the temperature at the bottom of the cryogenic cylinder 6 in real time and feeds the data back to the control system, achieving closed-loop temperature control, avoiding the risks of overheating or underheating, and ensuring the repeatability and safety of the reaction conditions.

[0034] A water-cooled block 101 is installed at the heat dissipation end of the thermoelectric cooler 3, efficiently dissipating heat through circulating coolant to maintain the cooling performance and service life of the thermoelectric cooler 3. The cryogenic protective shell 7, sealing ring 8, and sealing ring 14 form a double sealing barrier, effectively isolating external air and moisture from entering the cryogenic cylinder 6, preventing condensation or frost, and ensuring an undisturbed reaction environment. An insulation layer 9 covers the outer perimeter of the cryogenic cylinder 6, reducing heat exchange with the external environment, minimizing energy loss, and further improving cooling efficiency.

[0035] Meanwhile, the magnetic stirring system drives the magnet block 13 to rotate via the rotating motor 11, generating a rotating magnetic field that attracts the magnetic stir bar inside the reaction vessel 4 to rotate synchronously, achieving continuous and uniform mixing of the reactants and promoting reaction kinetics and heat conduction. The overall device has a compact structure and modular design, facilitating parallel operation and independent temperature control of multiple reaction systems, and is suitable for low-temperature high-throughput screening and optimization of reaction conditions in fields such as organic synthesis and drug development.

[0036] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A low-temperature reaction apparatus, characterized in that, The device includes a bracket (1), a mounting base (2), a thermoelectric cooler (3), and a reaction vessel (4). The mounting base (2) is fixedly mounted on the bracket (1). The reaction vessel (4) is mounted on the top of the mounting base (2). The thermoelectric cooler (3) is mounted on the bottom surface of the reaction vessel (4). The mounting base (2) is provided with a heat sink (10) for dissipating heat from the thermoelectric cooler (3).

2. The low-temperature reaction apparatus according to claim 1, characterized in that, The mounting base (2) is provided with a low temperature cylinder (6) on top. The low temperature cylinder (6) is fixedly mounted on the mounting base (2). The reaction vessel (4) is installed inside the low temperature cylinder (6). The semiconductor cooling chip (3) is installed on the bottom surface of the low temperature cylinder (6).

3. The low-temperature reaction apparatus according to claim 2, characterized in that, A low-temperature protective shell (7) is provided on the low-temperature cylinder (6), and a sealing ring (8) is provided at one end of the protective shell. The low-temperature protective shell (7) is sleeved on the outer periphery of the low-temperature cylinder (6), and the sealing ring (8) is located above the low-temperature cylinder (6). The inner wall of the sealing ring (8) abuts against the outer periphery of the reaction vessel (4), and a sealing ring (14) is provided between the sealing ring (8) and the top of the low-temperature cylinder (6).

4. The low-temperature reaction apparatus according to claim 3, characterized in that, The low-temperature cylinder (6) is provided with a heat insulation layer (9) around its outer peripheral wall, and the heat insulation layer (9) is located between the low-temperature cylinder (6) and the low-temperature protective shell (7).

5. A low-temperature reaction apparatus according to claim 4, characterized in that, The low-temperature cylinder (6) has an installation groove (61) on its bottom surface, and the semiconductor cooling chip (3) is embedded in the installation groove (61). The bottom surface of the low-temperature cylinder (6) has clearance grooves (62) on both sides of the installation groove (61) along its length, and the depth of the clearance grooves (62) is greater than that of the installation groove (61).

6. A low-temperature reaction apparatus according to claim 4, characterized in that, The bottom surface of the low-temperature cylinder (6) is also provided with a fixing groove (63), and a temperature sensor is installed in the fixing groove (63).

7. A low-temperature reaction apparatus according to claim 1, characterized in that, The heat dissipation component (10) is a water-cooled block (101). The water-cooled block (101) is installed on the heat dissipation end of the semiconductor cooling chip (3). The water-cooled block (101) has a flow channel inside. The water-cooled block (101) is provided with an inlet connector (1011) and an outlet connector (1012) for communicating with both ends of the flow channel.

8. A low-temperature reaction apparatus according to claim 1, characterized in that, A rotating motor (11) is provided below the mounting base (2). The rotating motor (11) is fixedly mounted on the bracket (1). The output end of the rotating motor (11) faces upward. A mounting plate (12) is provided at the output end of the rotating motor (11). Magnet blocks (13) are fixedly mounted at both ends of the top surface of the mounting plate (12) along the length direction.

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