A continuous photoreactor for the production of pharmaceutical intermediates

Abstract

The utility model relates to the technical field of pharmaceutical synthesis production, and disclose a kind of for the continuous photoreactor of pharmaceutical intermediate production, including box, box lower end four corners are uniformly connected with support leg, the left and right sides of box front end are uniformly provided with observation window, the box front end between two observation windows is fixedly connected with controller, box right end is fixedly connected with power cord, and power cord and controller are electrically connected;It also includes: photoreaction mechanism, photoreaction mechanism is installed in the inside of box.The utility model discloses by coaxial sleeve setting first helical reaction tube and second helical reaction tube in the outer side of lamp tube and up-down superposition intercommunication, reaction liquid flow distance is doubled to extend under the premise of not increasing equipment floor area, illumination time is significantly increased;While spiral structure makes reaction liquid whole course close to light source, and illumination uniformity is greatly promoted, thereby effectively improve the conversion rate and selectivity of pharmaceutical intermediate, and the occurrence of side reaction is inhibited.

Description

Technical Field

[0001] This utility model relates to the field of pharmaceutical synthesis and production technology, and in particular to a continuous photoreactor for the production of pharmaceutical intermediates. Background Technology

[0002] The photochemical synthesis of pharmaceutical intermediates needs to be completed under light of a specific wavelength. The contact time and contact area between the reactants and the light source directly determine the yield and selectivity of the product. Continuous photoreactors, by realizing continuous input, continuous reaction and continuous collection of materials, have become the mainstream development direction in this field.

[0003] Currently, most commonly used continuous photoreactors are composed of straight cylindrical or single-coil quartz tubes. The reaction liquid is pumped and passes through the illumination zone in a laminar or turbulent flow in one go. In order to obtain sufficient reaction time, the optical path can usually only be increased by extending the tube length.

[0004] However, as the tube length increases, the overall size of the equipment increases rapidly, and the floor space required increases significantly. At the same time, the reaction liquid far from the light source area is difficult to be uniformly illuminated due to the attenuation of light intensity, resulting in a decrease in reaction efficiency and an increase in side reactions, which restricts industrial scale-up applications. Utility Model Content

[0005] In order to overcome the above-mentioned defects of the prior art, this utility model provides a continuous photoreactor for the production of pharmaceutical intermediates, so as to solve the problems of insufficient illumination time due to short reaction paths, and the problem that simply extending the tube length makes the equipment bulky and the illumination uniformity poor.

[0006] This utility model provides a continuous photoreactor for the production of pharmaceutical intermediates, comprising a housing, with support legs fixedly connected to the four corners of the lower end of the housing, observation windows on both the left and right sides of the front end of the housing, a controller fixedly connected to the front end of the housing between two of the observation windows, and a power cord fixedly connected to the right end of the housing, the power cord being electrically connected to the controller; further comprising:

[0007] A light-reaction mechanism, which is installed inside the housing;

[0008] A cooling mechanism is installed at the bottom of the box body.

[0009] Preferably, the photoreaction mechanism includes reaction components and lamp tubes. Lamp holders are fixedly connected to the left and right sides of the top of the box. A pair of lamp tubes are provided and fixedly connected to the lower end of the lamp holders. A pair of reaction components are provided and symmetrically sleeved on the outer wall of the lamp tubes.

[0010] Preferably, the reaction assembly includes a first spiral reaction tube and a second spiral reaction tube coaxially sleeved on the outside of the lamp tube and distributed in parallel vertically. The upper end of the first spiral reaction tube is fixedly connected to a first connecting tube, and the end of the first connecting tube is fixedly connected to the upper end of the second spiral reaction tube.

[0011] Preferably, a second connecting pipe is fixedly connected to the lower end of the second spiral reaction tube located on the right side of the housing. The end of the second connecting pipe is fixedly connected to the lower end of the second spiral reaction tube on the left side of the housing. A third connecting pipe is fixedly connected inside the housing. The sidewalls of the third connecting pipe are respectively fixedly connected to the lower ends of the first spiral reaction tube. Both ends of the third connecting pipe extend to the outer wall of the housing. A gear pump is fixedly connected to the middle of the third connecting pipe. The gear pump is fixedly connected to the bottom of the housing through a fixing bracket. Both the left and right ends of the third connecting pipe are fixedly connected to first control valves. A second control valve is fixedly connected inside the third connecting pipe between the two first control valves. The interface between the first spiral reaction tube and the third connecting pipe is located between the first control valve and the second control valve.

[0012] Preferably, a temperature sensor is fixedly connected inside the second connecting tube, and the temperature sensor is electrically connected to the controller via a wire.

[0013] Preferably, the cooling mechanism includes a motor and a thermoelectric cooler. A pair of mounting holes are provided on the lower end face of the housing, located directly below the lamp tube. The mounting holes have chamfered edges. A pair of thermoelectric coolers are fixedly connected inside the mounting holes. Fins are fixedly connected to the upper end of each thermoelectric cooler. The motor is fixedly connected to the bottom of the housing via a mounting bracket, located directly above the thermoelectric cooler on the left side of the housing. A rotating shaft is also rotatably connected to the bottom of the housing via the mounting bracket, located directly above the thermoelectric cooler on the right side of the housing. The motor output shaft and the rotating shaft are connected via a pulley assembly. Fan blades are fixedly connected to the lower ends of both the motor output shaft and the rotating shaft. The motor and the thermoelectric cooler are electrically connected to the controller via wires.

[0014] Compared with the prior art, the beneficial effects of this utility model are:

[0015] 1. This utility model extends the flow distance of the reaction liquid by coaxially sleeved on the outside of the lamp tube and stacked and connected vertically without increasing the equipment floor space, thus significantly increasing the illumination time. At the same time, the spiral structure keeps the reaction liquid close to the light source throughout the process, greatly improving the uniformity of illumination, thereby effectively improving the conversion rate and selectivity of pharmaceutical intermediates and inhibiting the occurrence of side reactions.

[0016] 2. This utility model, by setting a cooling mechanism at the bottom of the chamber consisting of a semiconductor cooling chip, fins and forced convection fan blades, can remove the heat generated by the lamp tube and reaction liquid in real time, so as to keep the reaction temperature within the set range; the temperature sensor and controller are set in a closed loop to prevent overheating from causing side reactions and to avoid excessive cooling from reducing the reaction rate, thus ensuring the stability and safety of continuous production. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the overall main structure of this utility model;

[0018] Figure 2 This is a schematic diagram of the main cross-sectional structure of the box body of this utility model;

[0019] Figure 3 This is a rear view schematic diagram of the third connecting pipe of this utility model;

[0020] Figure 4 This is a schematic diagram of the exploded structure of the housing and cooling mechanism of this utility model.

[0021] Numbering on the map:

[0022] 1. Housing; 11. Observation window; 12. Support leg; 13. Power cord; 14. Controller; 15. Mounting hole; 16. Chamfer; 2. Photoreaction mechanism; 21. Reaction component; 211. First spiral reaction tube; 212. Second spiral reaction tube; 213. First connecting tube; 22. Second connecting tube; 23. Third connecting tube; 231. First control valve; 232. Second control valve; 24. Lamp holder; 25. Lamp tube; 26. Gear pump; 3. Temperature sensor; 4. Cooling mechanism; 41. Motor; 42. Shaft; 43. Fan blade; 44. Pulley assembly; 45. Semiconductor cooling chip; 46. Fin. Detailed Implementation

[0023] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.

[0024] like Figure 1-4 As shown, this utility model has the following two specific embodiments.

[0025] Example 1

[0026] A continuous photoreactor for the production of pharmaceutical intermediates includes a housing 1, with support legs 12 fixedly connected to the four corners of the lower end of the housing 1. Observation windows 11 are provided on both the left and right sides of the front end of the housing 1. A controller 14 is fixedly connected to the front end of the housing 1 between two observation windows 11. A power cord 13 is fixedly connected to the right end of the housing 1, and the power cord 13 is electrically connected to the controller 14. The device also includes:

[0027] Light reaction mechanism 2 is installed inside housing 1;

[0028] Cooling mechanism 4 is installed at the bottom of the box 1.

[0029] The light reaction mechanism 2 includes a reaction component 21 and a lamp tube 25. Lamp holders 24 are fixedly connected to the left and right sides of the top of the box 1. A pair of lamp tubes 25 are provided and fixedly connected to the lower end of the lamp holders 24. A pair of reaction components 21 are provided and symmetrically sleeved on the outer wall of the lamp tubes 25.

[0030] The reaction assembly 21 includes a first spiral reaction tube 211 and a second spiral reaction tube 212 coaxially sleeved on the outside of the lamp tube 25 and distributed in parallel vertically. A first connecting tube 213 is fixedly connected to the upper end of the first spiral reaction tube 211, and the end of the first connecting tube 213 is fixedly connected to the upper end of the second spiral reaction tube 212.

[0031] A second connecting pipe 22 is fixedly connected to the lower end of the second spiral reaction tube 212 located on the right side of the housing 1. The end of the second connecting pipe 22 is fixedly connected to the lower end of the second spiral reaction tube 212 on the left side of the housing 1. A third connecting pipe 23 is fixedly connected inside the housing 1. The side walls of the third connecting pipe 23 are fixedly connected to the lower end of the first spiral reaction tube 211. Both ends of the third connecting pipe 23 extend to the outer wall of the housing 1. A gear pump 26 is fixedly connected to the middle of the third connecting pipe 23. The gear pump 26 is fixedly connected to the bottom of the housing 1 through a fixing bracket. Both the left and right ends of the third connecting pipe 23 are fixedly connected to the first control valve 231. A second control valve 232 is fixedly connected inside the third connecting pipe 23 between the two first control valves 231. The interface between the first spiral reaction tube 211 and the third connecting pipe 23 is located between the first control valve 231 and the second control valve 232.

[0032] In this embodiment, as Figures 1-3 As shown, before starting, the target temperature and flow rate are set by the controller 14; at this time, the first control valve 231 is in the open state and the second control valve 232 is in the closed state to prevent the liquid from running dry.

[0033] The liquid to be reacted is injected from the left end of the third connecting pipe 23 until it fills the inner cavity of the first spiral reaction tube 211 and the second spiral reaction tube 212. Then, the controller 14 issues a command, the first control valve 231 closes, and the second control valve 232 opens, and the system enters the formal reaction stage: the lamp tube 25 is energized to produce light, and then the liquid, driven by the gear pump 26, flows sequentially through the left first spiral reaction tube 211 → left second spiral reaction tube 212 → second connecting pipe 22 → right second spiral reaction tube 212 → right first spiral reaction tube 211, and finally returns to the right end outlet of the third connecting pipe 23. Throughout the process, the liquid always spirals up or down close to the outer wall of the lamp tube 25, and the light path is significantly lengthened. The heat generated by the reaction is quickly discharged through the cooling mechanism 4.

[0034] After the reaction is completed, first shut off the gear pump 26 and the second control valve 232, then open the first control valve 231, and then inject inert gas from the left end of the third connecting pipe 23. Through the pressure difference, the residual liquid is returned to the external collection container from the right end of the third connecting pipe 23, thus completing one continuous photoreaction operation.

[0035] Example 2

[0036] The difference from Embodiment 1 is that this embodiment discloses a cooling mechanism 4 for cooling the photoreaction mechanism 2;

[0037] A temperature sensor 3 is fixedly connected inside the second connecting pipe 22. The temperature sensor 3 is electrically connected to the controller 14 via a wire.

[0038] The cooling mechanism 4 includes a motor 41 and a thermoelectric cooler 45. A pair of mounting holes 15 are provided on the lower end face of the housing 1, located directly below the lamp tube 25. A chamfer 16 is provided inside the mounting holes 15. A pair of thermoelectric coolers 45 are fixedly connected inside the mounting holes 15. Fins 46 are fixedly connected to the upper end of each thermoelectric cooler 45. The motor 41 is fixedly connected to the bottom of the housing 1 via a mounting bracket, located directly above the thermoelectric cooler 45 on the left side of the housing 1. A rotating shaft 42 is also rotatably connected to the bottom of the housing 1 via the mounting bracket. The rotating shaft 42 is located directly above the thermoelectric cooler 45 on the right side of the housing 1. The output shaft of the motor 41 and the rotating shaft 42 are connected via a pulley assembly 44. Fan blades 43 are fixedly connected to the lower ends of both the output shaft of the motor 41 and the rotating shaft 42. The motor 41 and the thermoelectric cooler 45 are electrically connected to the controller 14 via wires.

[0039] In this embodiment, as Figure 4As shown, two mounting holes 15 with chamfered edges 16 are symmetrically opened on the lower end face of the housing 1. A thermoelectric cooler 45 is embedded in each hole. The hot end of the cooler is close to the bottom plate of the housing 1, and the cold end faces upward and is welded with longitudinal fins 46. The fins 46 extend into the inner cavity of the housing 1, maintaining a safe distance from the lower end of the lamp tube 25 to avoid blocking the light path. The motor 41 is fixed on the mounting bracket directly above the left thermoelectric cooler 45, and the right thermoelectric cooler 45 is directly above the rotating shaft 42 horizontally mounted on the mounting bracket. The rotating shaft 42 is linked to the output shaft of the motor 41 by a synchronous belt pulley assembly 44. A centrifugal fan blade 43 is installed at the lower end of each shaft. The fan blade 43 is located at... Above the fins 46, air is drawn from the gaps between the fins 46 during rotation, causing the air to be discharged from bottom to top; the temperature sensor 3 collects the liquid temperature in the second connecting pipe 22 in real time and feeds it back to the controller 14; when the temperature exceeds the set upper limit, the controller 14 synchronously increases the speed of the motor 41 and increases the current of the semiconductor cooling chip 45 to achieve rapid cooling; when the temperature is below the lower limit, the controller 14 controls the motor 41 and the semiconductor cooling chip 45 to reduce power or operate intermittently to prevent overcooling; the entire cooling process does not require additional cooling medium, has a compact structure, low noise, and forms an efficient thermal management closed loop with the photo-reaction mechanism 2, ensuring the stability of continuous production.

[0040] The working principle of this utility model is as follows:

[0041] The pharmaceutical intermediate solution to be reacted is injected from the left end of the third connecting tube 23. Before injection, the controller 14 first opens the first control valve 231 and closes the second control valve 232, so that the liquid fills the double helix channel formed by the first helix reaction tube 211 and the second helix reaction tube 212. Then the first control valve 231 is closed and the second control valve 232 is opened, the gear pump 26 is started, and the liquid circulates along the closed path of "left first helix reaction tube 211 → left second helix reaction tube 212 → second connecting tube 22 → right second helix reaction tube 212 → right first helix reaction tube 211 → right end of the third connecting tube 23" at a constant flow rate. The light emitted by the lamp tube 25 directly irradiates the liquid through the quartz tube wall. The double helix structure greatly extends the optical path in a limited space, and the contact time and light-receiving area between the reactants and the light source are significantly increased, thereby improving the conversion rate and suppressing side reactions.

[0042] During the reaction, temperature sensor 3 monitors the liquid temperature in the second connecting pipe 22 in real time and feeds it back to controller 14. When the temperature is higher than the set value, controller 14 simultaneously increases the speed of motor 41 and the current of semiconductor cooling chip 45. Fan blade 43 rotates to quickly absorb the cold air between fins 46 and form a forced airflow from bottom to top, thereby reducing the temperature of the pharmaceutical intermediate solution. When the temperature is lower than the set value, controller 14 reduces power or operates intermittently to prevent overcooling. This closed-loop temperature control system does not require external cooling water, has a compact structure, low noise, and ensures that the reaction can proceed continuously under constant temperature conditions.

[0043] After the reaction is complete, the gear pump 26 stops, then the second control valve 232 is closed and the first control valve 231 is opened. Inert gas is introduced from the left end of the third connecting pipe 23, and the gas pressure is used to push all the residual liquid to the right end collection container. Then the lamp tube 25 is de-energized, and one continuous photochemical reaction operation is completed.

[0044] Although the disclosure is as stated above, the scope of protection of this disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of this disclosure, and all such changes and modifications will fall within the protection scope of this utility model.

Claims

1. A continuous photoreactor for the production of pharmaceutical intermediates, comprising a housing (1), characterized in that, Support legs (12) are fixedly connected to the four corners of the lower end of the box (1). Observation windows (11) are provided on the left and right sides of the front end of the box (1). A controller (14) is fixedly connected to the front end of the box (1) between two observation windows (11). A power cord (13) is fixedly connected to the right end of the box (1). The power cord (13) is electrically connected to the controller (14). The box (1) also includes: A light-reaction mechanism (2) is installed inside the housing (1); Cooling mechanism (4) is installed at the bottom of the box (1).

2. The continuous photoreactor for the production of pharmaceutical intermediates according to claim 1, characterized in that, The light reaction mechanism (2) includes a reaction component (21) and a lamp tube (25). The left and right sides of the top of the box (1) are fixedly connected to lamp holders (24). A pair of lamp tubes (25) are provided and fixedly connected to the lower end of the lamp holders (24). A pair of reaction components (21) are provided and symmetrically sleeved on the outer wall of the lamp tubes (25).

3. A continuous photoreactor for the production of pharmaceutical intermediates according to claim 2, characterized in that, The reaction assembly (21) includes a first spiral reaction tube (211) and a second spiral reaction tube (212) coaxially sleeved on the outside of the lamp tube (25) and distributed in parallel vertically. The upper end of the first spiral reaction tube (211) is fixedly connected to a first connecting tube (213), and the end of the first connecting tube (213) is fixedly connected to the upper end of the second spiral reaction tube (212).

4. A continuous photoreactor for the production of pharmaceutical intermediates according to claim 2, characterized in that, A second connecting pipe (22) is fixedly connected to the lower end of the second spiral reaction tube (212) located on the right side of the box (1). The end of the second connecting pipe (22) is fixedly connected to the lower end of the second spiral reaction tube (212) on the left side of the box (1). A third connecting pipe (23) is fixedly connected inside the box (1). The side walls of the third connecting pipe (23) are fixedly connected to the lower end of the first spiral reaction tube (211). Both ends of the third connecting pipe (23) extend to the outer wall of the box (1). A gear pump (26) is fixedly connected in the middle. The gear pump (26) is fixedly connected to the bottom of the box (1) through a fixing bracket. The left and right ends of the third connecting pipe (23) are fixedly connected to first control valves (231). The third connecting pipe (23) between the two first control valves (231) is fixedly connected to a second control valve (232). The interface between the first spiral reaction tube (211) and the third connecting pipe (23) is located between the first control valve (231) and the second control valve (232).

5. A continuous photoreactor for the production of pharmaceutical intermediates according to claim 4, characterized in that, A temperature sensor (3) is fixedly connected inside the second connecting tube (22), and the temperature sensor (3) is electrically connected to the controller (14) through a wire.

6. A continuous photoreactor for the production of pharmaceutical intermediates according to claim 1, characterized in that, The cooling mechanism (4) includes a motor (41) and a semiconductor cooling chip (45). A pair of mounting holes (15) are provided on the lower end face of the housing (1), located directly below the lamp tube (25). A chamfer (16) is provided inside each mounting hole (15). A pair of semiconductor cooling chips (45) are fixedly connected inside the mounting holes (15). A fin (46) is fixedly connected to the upper end of each semiconductor cooling chip (45). The motor (41) is fixedly connected to the bottom of the housing (1) via a mounting bracket. And located directly above the semiconductor cooling chip (45) on the left side of the housing (1), the bottom of the housing (1) is also rotatably connected to a rotating shaft (42) via a mounting bracket. The rotating shaft (42) is located directly above the semiconductor cooling chip (45) on the right side of the housing (1). The output shaft of the motor (41) and the rotating shaft (42) are connected by a pulley assembly (44). The lower ends of the output shaft of the motor (41) and the rotating shaft (42) are both fixedly connected to fan blades (43). The motor (41) and the semiconductor cooling chip (45) are both electrically connected to the controller (14) via wires.

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