Photochemical reactor and photochemical reaction method

Abstract

The present disclosure relates to the technical field of photochemical reaction, and particularly relates to a photochemical reactor and a photochemical reaction method. The photochemical reactor comprises: a module assembly box body, an inner part of the module assembly box body is provided with a sliding rail, the sliding rail extends along a first direction; a plurality of photochemical reaction modules located in the module assembly box body, the plurality of photochemical reaction modules are arranged along the first direction, and the plurality of photochemical reaction modules are movable along the sliding rail, and the plurality of photochemical reaction modules are used for sequentially absorbing photons emitted by a light source to perform photochemical reaction, wherein the first direction is parallel to a light direction of the light source. The present disclosure can efficiently solve the problem that the utilization efficiency of photons is attenuated with the progress of photochemical reaction, causing the photochemical reaction rate to slow down, the reaction time to be prolonged, and the overall energy consumption to be doubled.

Description

Technical Field

[0001] This disclosure relates to the field of photochemical reaction technology, and in particular to a photochemical reactor and a photochemical reaction method. Background Technology

[0002] Over the past decade, research and applications of photochemical reactions have experienced explosive growth, becoming a crucial tool for chemical bond construction. Compared to traditional thermochemical reactions, photochemical reactions can achieve highly selective and high-yield synthesis of target products under milder conditions, and are considered a key technology for advancing green chemistry and sustainable synthesis. As the core equipment for achieving photochemical conversion, the performance of the photochemical reactor directly determines the reaction efficiency and energy consumption level.

[0003] However, many types of photochemical reactors currently in widespread use, including internally illuminated batch reactors (such as CN102558272A), externally illuminated tubular reactors (such as CN218077848U), and microchannel reactors (such as CN218047860U and CN109806823A), all share a common technical bottleneck: they can only effectively act on thin layers of reaction solution with a limited thickness. During the reaction process, as the concentration of substrate molecules gradually decreases, their ability to capture photons decreases simultaneously, causing some photons to penetrate the reaction solution without being utilized, thus reducing photon utilization efficiency. This "substrate concentration-photon flux" mismatch not only wastes light energy but also slows down the reaction rate, prolongs the reaction time, and multiplies the overall energy consumption, severely restricting the economics and feasibility of photochemical technology in large-scale synthesis and industrial applications. Summary of the Invention

[0004] To address the aforementioned technical problems, this disclosure provides a photochemical reactor and a photochemical reaction method, which can effectively solve the problem of photon utilization efficiency decreasing as the photochemical reaction progresses, resulting in a slowdown in the photochemical reaction rate, a prolonged reaction time, and a significant increase in overall energy consumption.

[0005] In a first aspect, this disclosure provides a photochemical reactor, comprising: a modular assembly box, wherein a slide rail is provided inside the modular assembly box and extends along a first direction; a plurality of photochemical reaction modules located inside the modular assembly box, the plurality of photochemical reaction modules being arranged along the first direction and movable along the slide rail, the plurality of photochemical reaction modules being used to sequentially absorb photons emitted by a light source to carry out a photochemical reaction, wherein the first direction is parallel to the direction of the light emitted by the light source.

[0006] In some embodiments, the photochemical reaction module includes a reflux condenser, a condensate device, and a photochemical reaction pool; the photochemical reaction pool is used to contain the photochemical reaction liquid to be carried out; the condensate device is attached to and covers part of the outer wall of the photochemical reaction pool, and is used to control the temperature inside the photochemical reaction pool; the reflux condenser is connected in a continuous manner to the photochemical reaction pool, and is used to condense and reflux volatile solvents.

[0007] In some embodiments, the photochemical reaction cell has a flat, hollow, three-dimensional structure, and its largest area plane is perpendicular to the light emitted by the light source; one end of the photochemical reaction cell is provided with a connection port, and the reflux condenser is connected to the photochemical reaction cell through the connection port; a sampling port is provided at the edge of the photochemical reaction cell.

[0008] In some embodiments, a gas guide plate is provided in the photochemical reaction cell, and the gas guide plate is densely covered with gas guide holes; an air inlet is provided at the end of the photochemical reaction cell away from the connection port.

[0009] In some embodiments, the material of the photochemical reaction cell is a highly transparent material, and the thickness of the photochemical reaction cell along the first direction is 1-10 cm.

[0010] In some embodiments, the condensate device has a concave hollow three-dimensional structure. Along the first direction, the condensate device does not overlap with the photochemical reaction cell, and part of the condensate device is located between the reflux condensate device and the photochemical reaction cell. The condensate device has an outlet on the side near the reflux condensate device and an inlet on the side away from the reflux condensate device.

[0011] In some embodiments, the outer surface of the condensate device is provided with a slider that matches the slide rail.

[0012] In some embodiments, a condensate device is located between the reflux condenser and the photochemical reaction tank. The condensate device includes a first hole, and a connection port is located inside the first hole. The reflux condenser has an outlet on the side away from the connection port.

[0013] In some embodiments, the module assembly housing further includes a drive mechanism for driving multiple photochemical reaction modules to move along a slide rail.

[0014] Secondly, this disclosure provides a photochemical reaction method applied to the aforementioned photochemical reactor. The photochemical reaction method includes: placing multiple photochemical reaction modules loaded with photoreaction liquid into a module assembly box; turning on a light source, with photons emitted by the light source sequentially initiating the photochemical reaction of each chemical reaction module; after the photochemical reaction is completed in the photochemical reaction module closest to the light source, removing it from the module assembly box; moving other photochemical reaction modules in the module assembly box toward the direction closer to the light source; and adding a photochemical reaction module loaded with photoreaction liquid to the side of the module assembly box away from the light source.

[0015] The technical solution provided in this disclosure has the following advantages compared with the prior art: The photochemical reactor disclosed herein fundamentally solves the problem of ineffective photon penetration in the low-concentration stage of traditional photochemical reactors through a "photon penetration-multi-stage utilization" mechanism, extending light energy utilization from a single point to the entire process. It maintains a high-rate reaction throughout, avoiding the decrease in photoreaction rate caused by the mismatch between substrate molecule concentration and photon count in the photoreaction solution in the later stages of the reaction, thus significantly shortening the total reaction time and reducing energy consumption per unit product. The photochemical reaction module can be promptly removed from the light field after the reaction is complete, effectively preventing product decomposition or side reactions due to excessive light exposure, which helps improve the yield and purity of the target product. The modular design makes the photochemical reactor easy to scale up; processing capacity can be increased simply by increasing the number of photochemical reaction modules, avoiding the problem of decreased mass transfer and light transmission efficiency in traditional scale-up processes.

[0016] Correspondingly, the photochemical reaction method provided in this disclosure also has the above-mentioned technical effects. Attached Figure Description

[0017] The accompanying drawings, which are incorporated in and form a part of this specification, illustrate embodiments consistent with this disclosure and, together with the description, serve to explain the principles of this disclosure.

[0018] To more clearly illustrate the technical solutions in the embodiments of this disclosure or the prior art, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the structure of a photochemical reaction device provided in this disclosure; Figure 2 This is a schematic diagram of the structure of a photochemical reaction module provided in this disclosure; Figure 3 This is a schematic flowchart of a photochemical reaction method provided in this disclosure.

[0020] Reference numerals: 1. Module assembly box; 2. Photochemical reaction module; 11. Slide rail; 12. Side plate; 13. Base; 14. Support rod; 21. Condensation reflux device; 22. Condensate device; 23. Photochemical reaction tank; 211. Gas outlet; 221. Water inlet; 222. Water outlet; 223. Slider; 231. Air guide plate; 232. Air inlet; 233. Connection port. Detailed Implementation

[0021] To better understand the above-mentioned objectives, features, and advantages of this disclosure, the solutions disclosed herein will be further described below. It should be noted that, unless otherwise specified, the embodiments and features described herein can be combined with each other.

[0022] Numerous specific details are set forth in the following description in order to provide a full understanding of this disclosure, but this disclosure may also be implemented in other ways different from those described herein; obviously, the embodiments in the specification are only some, and not all, of the embodiments of this disclosure.

[0023] Figure 1 This is a schematic diagram of a photochemical reaction device provided in this disclosure, for reference. Figure 1 This disclosure provides a photochemical reactor, which includes: The module assembly box 1 has a slide rail 11 inside, which extends along the first direction X. Multiple photochemical reaction modules 2 are located inside the module assembly box 1. The multiple photochemical reaction modules 2 are arranged along the first direction X and can move along the slide rail 11. The multiple photochemical reaction modules 2 are used to sequentially absorb photons emitted by the light source to carry out photochemical reactions. The first direction X is parallel to the direction of the light emitted by the light source.

[0024] Specifically, this embodiment provides a photochemical reactor, which includes a modular assembly box 1 and multiple photochemical reaction modules 2 located within the modular assembly box 1. The photochemical reaction modules 2 are used to absorb photons emitted by a light source to perform a photochemical reaction. Multiple photochemical reaction modules 2 located within the module assembly box 1 are arranged along a first direction X, which is parallel to the direction of light emitted by the light source. This means that the multiple photochemical reaction modules 2 within the module assembly box 1 are arranged along the direction of light emitted by the light source. Consequently, the multiple photochemical reaction modules 2 within the module assembly box 1 can sequentially absorb photons emitted by the light source to carry out photochemical reactions. Specifically, when the substrate concentration in the photoreaction liquid of the photochemical reaction module 2 closest to the light source is the highest, it can efficiently absorb and utilize photons. As the photochemical reaction proceeds, the substrate concentration in the photoreaction liquid of the photochemical reaction module 2 closest to the light source gradually decreases. The photons that are not absorbed by this module are captured and utilized by the next photochemical reaction module 2. This process is passed sequentially, allowing photon energy to be utilized in a "relay" manner within multiple photochemical reaction modules 2, thereby significantly improving the overall photon utilization efficiency.

[0025] The module assembly box 1 is equipped with a slide rail 11 extending along the first direction X, allowing multiple photochemical reaction modules 2 to move along the slide rail 11. After the photochemical reaction in the photochemical reaction module 2 closest to the light source is completed, it can be removed from the module assembly box 1, and the other photochemical reaction modules 2 within the module assembly box 1 can be moved towards the light source. Subsequently, a new photochemical reaction module 2 loaded with photoreaction liquid can be added to the side of the module assembly box 1 away from the light source. This achieves dynamic rotation of the photochemical reaction modules 2 within the module assembly box 1, ensuring that at any reaction moment, photons emitted by the light source are always effectively captured by the photoreaction liquid, achieving optimized matching of "concentration-photon" throughout the process.

[0026] The photochemical reactor provided in this embodiment fundamentally solves the problem of ineffective photon penetration in the low-concentration stage of traditional photochemical reactors through the "photon penetration-multi-stage utilization" mechanism, extending the utilization of light energy from a single point to the entire process. It maintains a high-rate reaction throughout the process, avoiding the decrease in photoreaction rate caused by the mismatch between the substrate molecule concentration and the number of photons in the photoreaction liquid in the later stage of the reaction, thus significantly shortening the total reaction time and reducing the energy consumption per unit product. The photochemical reaction module 2 can be removed from the light field in a timely manner after the reaction is completed, effectively avoiding the decomposition or side reactions of the product due to excessive light exposure, which helps to improve the yield and purity of the target product. The modular design makes the photochemical reactor easy to scale up, and the processing capacity can be increased simply by increasing the number of photochemical reaction modules 2, avoiding the problem of decreased mass transfer and light transmission efficiency in the traditional scale-up process.

[0027] It should be noted that, Figure 1The example shown in this disclosure illustrates that four photochemical reaction modules 2 are provided inside the module assembly box 1. In other embodiments of this disclosure, the number of photochemical reaction modules 2 inside the module assembly box 1 can be other values, which can be set according to the requirements. This disclosure will not elaborate on them here.

[0028] Figure 2 This is a schematic diagram of the structure of a photochemical reaction module provided in this disclosure, for reference. Figure 1 and Figure 2 In some embodiments, the photochemical reaction module 2 includes a reflux condenser 21, a condensate device 22, and a photochemical reaction tank 23; Photochemical reaction tank 23 is used to contain the photochemical reaction liquid to be carried out; The condensate device 22 is attached to and covers part of the outer wall of the photochemical reaction tank 23. The condensate device 22 is used to control the temperature inside the photochemical reaction tank 23. The reflux condenser 21 is connected in series with the photochemical reaction cell 23. The reflux condenser 21 is used to condense and reflux volatile solvents.

[0029] Specifically, the photochemical reaction module 2 includes a reflux condenser 21, a condensate system 22, and a photochemical reaction tank 23. The photochemical reaction tank 23 is used to contain the photoreaction liquid to be used in the photochemical reaction; that is, the photochemical reaction tank 23 serves as a place to contain the photoreaction liquid and provide a site for the photochemical reaction. The condensate system 22 is attached to and covers part of the outer wall of the photochemical reaction tank 23. The condensate system 22 is used to control the temperature inside the photochemical reaction tank 23, thereby controlling the temperature at which the photochemical reaction takes place. The reflux condenser 21 is connected to the photochemical reaction tank 23 and is used to condense and reflux the solvent that evaporates during the photochemical reaction. In other words, the photochemical reaction module 2 is an independent unit integrating reaction, temperature control, and reflux functions.

[0030] Continue to refer to Figure 1 and Figure 2 In some embodiments, the photochemical reaction cell 23 has a flat, hollow, three-dimensional structure, and its largest area plane is perpendicular to the light emitted by the light source. One end of the photochemical reaction cell 23 is provided with a connection port 233, and the reflux condenser 21 is connected to the photochemical reaction cell 23 through the connection port 233. A sampling port (not shown in the figure) is provided at the edge of the photochemical reaction cell 23.

[0031] Specifically, the photochemical reaction cell 23 has a flat, hollow, three-dimensional structure, and its largest plane is perpendicular to the light emitted by the light source. This allows the light from the light source to be incident perpendicularly on its largest plane, which is beneficial for the photochemical reaction liquid in the photochemical reaction cell 23 to absorb photons and carry out photochemical reactions.

[0032] One end of the photochemical reaction cell 23 is provided with a connection port 233. The reflux condenser 21 is connected to the photochemical reaction cell 23 through the connection port 233, so that the solvent volatilized during the photochemical reaction can be condensed and refluxed back to the photochemical reaction cell 23 through the reflux condenser 21.

[0033] The edge of the photochemical reaction cell 23 is provided with a sampling port, through which the photochemical reaction liquid in the photochemical reaction cell 23 can be sampled, thereby enabling real-time detection of the photochemical reaction process.

[0034] Continue to refer to Figure 1 and Figure 2 In some embodiments, a gas guide plate 231 is provided in the photochemical reaction cell 23, and the gas guide plate 231 is densely covered with gas guide holes. An air inlet 232 is provided at the end of the photochemical reaction tank 23 away from the connection port 233.

[0035] Specifically, the photochemical reaction cell 23 has an air inlet 232 at the end furthest from the connection port 233, through which inert gas (such as nitrogen or argon) or reactive gas can be introduced into the photochemical reaction cell 23. The photochemical reaction cell 23 also has a gas guide plate 231, which can be connected to the air inlet 232. The gas guide plate 231 is densely covered with gas guide holes. When inert gas or reactive gas is introduced into the photochemical reaction cell 23 through the air inlet 232, the gas guide plate 231 can evenly distribute the inert gas or reactive gas into the photoreaction liquid, while simultaneously agitating the photoreaction liquid to achieve the purpose of homogenizing the photoreaction system.

[0036] Continue to refer to Figure 1 and Figure 2 In some embodiments, the material of the photochemical reaction cell 23 is a high-transmittance material, and the thickness of the photochemical reaction cell 23 along the first direction X is 1-10cm.

[0037] Specifically, the photochemical reaction cell 23 is made of a high-transmittance material, which reduces the attenuation of light during propagation and ensures that the incident light fully enters the photochemical reaction cell 23, facilitating the absorption of photons by the photoreaction liquid within the cell and enabling the photochemical reaction. Optionally, the material of the photochemical reaction cell 23 can be high-transmittance borosilicate glass or quartz glass. Of course, the material of the photochemical reaction cell 23 can also be other high-transmittance materials, which will not be elaborated upon here.

[0038] Along the first direction X, the thickness of the photochemical reaction cell 23 is 1-10 cm to ensure that the photoreactive liquid within the cell forms an optimized thin layer, which is beneficial for the photoreactive liquid in the cell to absorb photons and carry out the photochemical reaction. Simultaneously, it avoids the photochemical reaction cell 23 being too thin, which simplifies the process and reduces production costs. Optionally, along the first direction X, the thickness of the photochemical reaction cell 23 is 1-4 cm to ensure that the photoreactive liquid within the cell forms an even more optimized thin layer, which is beneficial for the photoreactive liquid in the cell to absorb photons and carry out the photochemical reaction.

[0039] Continue to refer to Figure 1 and Figure 2 In some embodiments, the structure of the condensate device 22 is a concave hollow three-dimensional structure. Along the first direction X, the condensate device 22 does not overlap with the photochemical reaction cell 23, and part of the condensate device 22 is located between the reflux condensate device 21 and the photochemical reaction cell 23. The condensate device 22 has an outlet 222 on the side close to the return condensate device 21 and an inlet 221 on the side away from the return condensate device 21.

[0040] Specifically, the condensate device 22 has a concave, hollow, three-dimensional structure. Part of the condensate device 22 is located between the reflux condenser 21 and the photochemical reaction tank 23, pointing from the reflux condenser 21 towards the photochemical reaction tank 23. The condensate device 22 is inverted at one end of the photochemical reaction tank 23, and can adhere to and cover part of the outer wall of the photochemical reaction tank 23. The condensate device 22 has an outlet 222 on the side near the reflux condenser 21 and an inlet 221 on the side away from the reflux condenser 21. The condensate can enter the condensate device 22 through the inlet 221 and flow out through the outlet 222. The condensate in the condensate device 22 can exchange heat with the photochemical reaction tank 23, thereby controlling the temperature inside the photochemical reaction tank 23 and thus controlling the temperature of the photochemical reaction.

[0041] Optionally, the condensate device 22 can be made of aluminum alloy.

[0042] Along the first direction X, the condensate device 22 does not overlap with the photochemical reaction cell 23, that is, the condensate device 22 will not cover the plane with the largest area in the photochemical reaction cell 23, so the setting of the condensate device 22 will not affect the light rays shining into the photochemical reaction cell 23.

[0043] Continue to refer to Figure 1 and Figure 2 In some embodiments, the outer surface of the condensate device 22 is provided with a slider 223 that matches the slide rail 11.

[0044] Specifically, a slider 223 is provided on the outer side of the condensate device 22. The structure of the slider 223 can be matched with the structure of the slide rail 11. The slider 223 can move along the slide rail 11. The slider 223 drives the condensate device 22 to move along the slide rail 11, thereby driving the photochemical reaction module 2 as a whole to move along the slide rail 11, thus realizing the movement of the photochemical reaction module 2 along the slide rail 11.

[0045] It should be noted that this disclosure does not specifically limit the structure of the slide rail 11 and the slider 223. The structure of the slider 223 can be matched with the structure of the slide rail 11. The movement of the slider 223 can drive the entire photochemical reaction module 2 to move along the slide rail 11. This disclosure will not elaborate further here.

[0046] Continue to refer to Figure 1 and Figure 2 In some embodiments, the condensate device 22 is located between the reflux condensate device 21 and the photochemical reaction tank 23. The condensate device 22 includes a first hole, and the connection port 233 is located inside the first hole. The reflux condenser 21 has an outlet 211 on the side away from the connection port 233.

[0047] Specifically, the condensate device 22 is located between the reflux condenser 21 and the photochemical reaction tank 23. The condensate device 22 has a first hole, and the connection port 233 is located within this first hole. This allows the reflux condenser 21 to be connected to the photochemical reaction tank 23 via the connection port 233, enabling the solvent volatilized during the photochemical reaction to be condensed and returned to the photochemical reaction tank 23 via the reflux condenser 21. An outlet 211 is located on the side of the reflux condenser 21 furthest from the connection port 233, allowing gas from the photochemical reaction tank 23 to be discharged through the reflux condenser 21 and the outlet 211.

[0048] Continue to refer to Figure 1 and Figure 2 In some embodiments, the module assembly box 1 also includes a drive mechanism (not shown in the figure), which is used to drive multiple photochemical reaction modules 2 to move along the slide rail 11. In other words, the multiple photochemical reaction modules 2 can be driven to move in conjunction along the slide rail 11 by the drive mechanism, thereby realizing the movement of multiple photochemical reaction modules 2 along the slide rail 11.

[0049] Optionally, the driving mechanism may include a stepper motor-driven push rod system, thereby driving the photochemical reaction module 2 to move synchronously and precisely along the slide rail 11. Of course, in other embodiments of this disclosure, the driving mechanism may also include other driving mechanisms, which will not be described in detail here.

[0050] Continue to refer to Figure 1 and Figure 2 In some embodiments, the module assembly housing 1 further includes two opposing side plates 12, a base 13 connected between the two side plates 12, and a support rod 14. The side plates 12, base 13, and support rod 14 form a cavity for accommodating the photochemical reaction module 2. The light inlet formed by the side plates 12 and base 13 is opposite to the support rod 14, allowing light from a light source to enter the photochemical reaction module 2 located inside the module assembly housing 1 through the light inlet. The first inlet formed by the side plates 12 and support rod 14 is opposite to the base 13, allowing the photochemical reaction module 2 to be placed into the module assembly housing 1 through the first inlet.

[0051] Optionally, the slide rail 11 can be mounted on the side plate 12. Correspondingly, the slider 223, which matches the slide rail 11, is mounted on the outer side of the condensate device 22 at the position corresponding to the side plate 12, thereby enabling the slider 223 to be positioned and moved on the slide rail 11.

[0052] It should be noted that in other embodiments of this disclosure, the slide rail 11 can also be set at other positions of the module assembly box 1. For example, the slide rail 11 can also be set on the base 13. Correspondingly, the structure of the condensate device 22 is also adapted, and the position of the slider 223 that matches the slide rail 11 is also adapted. This disclosure will not elaborate further here.

[0053] This disclosure provides a photochemical reaction method applied to the aforementioned photochemical reactor. Figure 3 This is a schematic flowchart of a photochemical reaction method provided in this disclosure, for reference. Figure 3 Photochemical reaction methods include: Step S100: Place multiple photochemical reaction modules containing photoreaction liquid into the module assembly box; Step S200: Turn on the light source. The photons emitted by the light source sequentially initiate the photochemical reactions of each chemical reaction module. Step S300: After the photochemical reaction is completed in the photochemical reaction module with the shortest distance from the light source, remove it from the module assembly box; Step S400: Move other photochemical reaction modules inside the module assembly box toward the direction of the light source; Step S500: Add a photochemical reaction module containing a photoreaction liquid to the side of the module assembly box away from the light source.

[0054] Specifically, in combination Figure 1 and Figure 3The photochemical reaction method provided in this embodiment is applied to a photochemical reactor. The photochemical reactor includes a modular assembly box 1 and multiple photochemical reaction modules 2 located within the modular assembly box 1. The photochemical reaction modules 2 are used to absorb photons emitted by a light source to carry out a photochemical reaction. Multiple photochemical reaction modules 2 located within the module assembly housing 1 are arranged along a first direction X, which is parallel to the optical path of the light emitted by the light source. This means the modules 2 are aligned with the direction of the light emitted by the light source, allowing them to sequentially absorb photons emitted by the light source and undergo photochemical reactions. Specifically, the module 2 closest to the light source has the highest substrate concentration in its photoreaction solution, enabling it to efficiently absorb and utilize photons. As the photochemical reaction progresses, the substrate concentration in the photoreaction solution of the module 2 closest to the light source gradually decreases. Unabsorbed photons are captured and utilized by the next module 2, and this process continues sequentially, allowing photon energy to be utilized in a relay-like manner across multiple modules 2, significantly improving the overall photon utilization efficiency. Furthermore, the module assembly housing 1 is equipped with a slide rail 11 extending along the first direction X, allowing the multiple photochemical reaction modules 2 to move along it.

[0055] In the photochemical reaction method provided in this embodiment, multiple photochemical reaction modules 2 loaded with photoreaction liquid are first placed inside the module assembly box 1. When the light source is turned on, the photons emitted by the light source first initiate the photochemical reaction of the first photochemical reaction module 2 (the photochemical reaction module 2 closest to the light source). When the photochemical reaction of the first photochemical reaction module 2 reaches a certain extent, the substrate molecule concentration decreases, resulting in a photon surplus. At this point, the photons enter the second photochemical reaction module 2 to initiate the photochemical reaction of that module, and so on, with photons entering subsequent photochemical reaction modules 2 to initiate the photochemical reaction. Once the photochemical reaction in the photochemical reaction module 2 closest to the light source is completed, it is removed from the module assembly box 1. Then, the other photochemical reaction modules 2 in the module assembly box 1 are moved toward the light source. After that, a new photochemical reaction module loaded with photoreaction liquid is added to the side of the module assembly box 1 away from the light source. The above steps are repeated to realize the dynamic rotation of the photochemical reaction modules 2 in the module assembly box 1, complete the continuous or semi-continuous photochemical reaction, and ensure that at any reaction moment, the photons emitted by the light source can always be effectively captured by the photoreaction liquid, so as to achieve the full-process optimized matching of "concentration-photon".

[0056] The photochemical reaction method provided in this embodiment is applied to the photochemical reactor provided in this disclosure embodiment. Through the "photon penetration-multi-stage utilization" mechanism, it fundamentally solves the problem of ineffective photon penetration in the low-concentration stage of traditional photochemical reactors, extending the utilization of light energy from a single point to the entire process. It maintains a high-rate photoreaction throughout the process, avoiding the rate drop in the later stage of the photoreaction, thus significantly shortening the total reaction time and reducing the energy consumption per unit product. The photochemical reaction module 2 can be removed from the light field in a timely manner after the reaction is completed, effectively avoiding the decomposition or side reactions of the product due to excessive light exposure, which helps to improve the yield and purity of the target product. The modular design makes the photochemical reactor easy to scale up. The processing capacity can be increased simply by increasing the number of photochemical reaction modules 2, avoiding the problem of decreased mass transfer and light transmission efficiency in the traditional scale-up process.

[0057] In some optional embodiments, the photochemical reaction method provided in this embodiment further includes: Prepare a photoreaction solution of a predetermined concentration; An inert gas (such as nitrogen or argon) is introduced into the photochemical reaction cell 23 through the air inlet 232 at the bottom to replace and remove air from the reaction system. After the gas replacement is complete, the prepared photoreaction liquid is transferred into the photochemical reaction cell 23 through the connection port 233, and slow, continuous aeration is maintained. The photochemical reaction tank 23, the condensate device 22, and the reflux condenser 21, which have been filled with liquid, are assembled into a complete photochemical reaction module 2; Multiple photochemical reaction modules 2 are stacked one after the other and loaded into the module assembly box 1 by the cooperation of slider 223 and slide rail 11; The circulation system of the condensate device 22 and the reflux condenser 21 is turned on to pre-cool and control the temperature of the reaction system; Once the temperature of the photoreaction liquid in each photochemical reaction module 2 is constant and the aeration is stable, the light source is activated to carry out the photochemical reaction. In the initial stage of the reaction, the substrate concentration of the photoreaction liquid in the first photochemical reaction module 2 (M1) at the forefront is the highest, which can efficiently absorb and utilize most of the incident photons, and the reaction proceeds rapidly. As the reaction progresses, the substrate concentration of the photoreaction liquid in module M1 gradually decreases. When the concentration is too low to completely capture photons, the photons that have passed through enter the next photochemical reaction module 2 (M2), where they are effectively captured by the photoreaction liquid with a higher substrate concentration. This initiates and maintains the photochemical reaction in module M2. This "photon penetration-cascade utilization" process is passed on sequentially. During this process, samples are taken periodically through the sampling port 234 of each chemical reaction module 2, and the reaction process in each chemical reaction module 2 is monitored in real time using analytical methods such as high performance liquid chromatography (HPLC). When the monitoring data shows that the substrate conversion rate of the photochemical reaction liquid in the first photochemical reaction module 2 (M1) reaches the predetermined endpoint (e.g., >98%), the illumination of the module is stopped and it is removed from the front end of the optical path of the module assembly box 1. Start the drive mechanism of the module assembly box 1, so that all the remaining photochemical reaction modules 2 (M2, M3, ...) move forward one station synchronously along the slide rail 11 as a whole. At this time, the original M2 module becomes the new first photochemical reaction module 2. At the empty workstation at the end of module assembly box 1, a new photochemical reaction module (Mn) loaded with fresh photoreaction liquid is added. This operation ensures that the light path is always effectively utilized, and photons do not needlessly penetrate the entire reaction system, thus achieving efficient utilization of light energy throughout the process.

[0058] The photoreaction liquid removed from the photochemical reaction module 2 (after the reaction has been completed) is poured out for subsequent separation and purification. The vacated photochemical reaction module 2, after cleaning and drying, can be refilled with photoreaction liquid and added to the end of the system in subsequent cycles, thus achieving the cyclical and continuous operation of the reactor.

[0059] Through repeated cycles of the above steps, the photochemical reaction method provided in this disclosure achieves efficient and energy-saving continuous photochemical reactions while maintaining high photon utilization and high reaction rate.

[0060] Exemplary, this embodiment provides a specific example of synthesizing compound P using the above-described photochemical reactor: Step 1, reaction preparation and module initialization: ① At 25°C, dissolve 50 g of ergosterol and 35 mg of di-tert-butylmethoxyphenol in 2 liters of a mixed solvent of n-hexane and methanol (volume ratio 6:1) and stir thoroughly to prepare a homogeneous raw material solution.

[0061] ② Introduce nitrogen gas into each of the four photochemical reaction cells 23 for 10 minutes to completely replace and remove oxygen from the system. Then, precisely add 400 ml of the prepared ergosterol feed solution to each photochemical reaction cell 23, and maintain a slow and steady nitrogen flow.

[0062] Step 2, Module Assembly and System Startup: ① The four photochemical reaction tanks 23, which have been filled with liquid and nitrogen, are assembled with the corresponding condensate device 22 and reflux condensate device 21 to form four independent photochemical reaction modules 2.

[0063] ② Load these four modules one on top of the other onto the slide rail 11 of the module assembly box 1. Turn on the condensate circulation system and reflux condensation system of all modules to ensure that the reaction temperature is controllable.

[0064] The third step, photo-reaction initiation and module dynamic rotation: ① Once the temperature of the ergosterol feedstock solution in all photochemical reaction tanks 23 has stabilized at 25℃±1℃ and the nitrogen bubbling has been stable, start the LED surface light source with a center wavelength of 280 nm and a power of 50 watts to initiate the photochemical reaction.

[0065] In the initial stage of the reaction, the light is efficiently absorbed by the first photochemical reaction module 2 (M1) at the forefront.

[0066] As the reaction proceeds, at a specific point in time, photons begin to penetrate module M1 and are effectively utilized by the second photochemical reaction module 2 (M2), marking the successful initiation of the "photon cascade utilization" mechanism.

[0067] ② Samples are taken through sampling port 234 of module M1, and the reaction process is monitored using high-performance liquid chromatography (HPLC).

[0068] ③ Seven minutes after the reaction started, HPLC analysis showed that the conversion rate of ergosterol in module M1 had exceeded 98.2%, reaching the reaction endpoint. Module M1 was then removed from the front of the optical path.

[0069] ④ At the same time, the drive mechanism of module assembly box 1 is activated, causing the remaining M2, M3 and M4 modules to move forward one station as a whole (M2 becomes the new first module), and a new module (M5) containing 400 ml of fresh ergosterol raw material solution is added at the end of the system.

[0070] Step 4: Continuous operation and product collection: Following the aforementioned dynamic rotation pattern, the system operates continuously. Subsequent modules reach the reaction endpoint and are removed from the system sequentially at 12 minutes, 16 minutes, 19.5 minutes, and 23 minutes after the reaction begins, respectively. After each module is removed, the photoreaction liquid within it is immediately poured out and collected.

[0071] Step 5, Post-processing and Result Analysis: ① All collected photoreaction solutions were combined and concentrated under reduced pressure to remove the solvent, yielding the photo-irradiated intermediate previtamin D2 and photo-irradiated byproducts. HPLC analysis showed that the conversion rate of the raw material ergosterol was as high as 97.5%.

[0072] ② Subsequently, the obtained intermediate pre-vitamin D2 and light-induced byproducts were subjected to a thermal isomerization reaction under specific conditions to obtain crude vitamin D2. Quantitative analysis of the crude product showed that the molar percentage of vitamin D2 was 63.7%.

[0073] In addition, this disclosure also provides comparative examples of the synthesis of compound P using a photochemical reactor provided by related technology: Comparative Example 1 Compared with the above-described embodiments of the present disclosure, the equipment used in this comparative embodiment is completely identical to that in the above-described embodiments of the present disclosure, except that it adopts a mode in which each of the five photochemical reaction modules is individually illuminated.

[0074] Five photoreaction modules were removed from the photoreaction system at 7 minutes, 15 minutes, 22 minutes, 30 minutes, and 38 minutes, respectively. All collected photoreaction solutions were combined and concentrated under reduced pressure to remove the solvent, yielding the photo-irradiated intermediate pre-vitamin D2 and photo-irradiated byproducts. HPLC analysis showed that the conversion rate of the starting material ergosterol was 93.7%.

[0075] After the thermal isomerization reaction of previtamin D2 and light-induced byproducts, the molar percentage of vitamin D2 in the crude product was 61.5%.

[0076] Comparative Example 2 Compared with the embodiments disclosed above, this comparative embodiment uses a batch-type photoreactor, in which 2L of ergosterol raw material solution is placed in a single 3.5L batch-type photoreactor for photoreaction. The photoreaction conditions are completely consistent with those of the embodiments disclosed above.

[0077] At 57 minutes after the start of the reaction, HPLC analysis showed that the conversion rate of ergosterol in the batch photoreactor exceeded 95.3%, at which point the reaction was terminated. All collected photoreaction solutions were combined and concentrated under reduced pressure to remove the solvent, yielding the photo-induced intermediate previtamin D2 and photo-induced byproducts.

[0078] After the thermal isomerization reaction of previtamin D2 and light-induced byproducts, the molar percentage of vitamin D2 in the crude product was 32.3%.

[0079] The above-described embodiments of this disclosure successfully utilized the photochemical reactor provided in this disclosure to achieve the conversion of ergosterol to vitamin D2. Compared with Comparative Examples 1 and 2, the results show that this disclosure has significant advantages: High efficiency and continuous operation: It achieves near-"assembly line" continuous light synthesis, with the shortest interval between individual modules being only about 3.5 minutes, which greatly improves the time and space productivity of the equipment.

[0080] Highly efficient use of photons: Through module rotation and photon penetration utilization mechanism, it is ensured that light energy is fully captured throughout the reaction process, which is the key to achieving efficient conversion of raw materials (ergosterol conversion rate exceeds 97% within 23 minutes).

[0081] Excellent product quality: Timely removal of the reaction module after the reaction was completed effectively avoided the excessive photodecomposition of the highly active intermediate M, laying a solid foundation for obtaining the high-purity target product P (63.7%) in subsequent steps.

[0082] The above-described embodiments powerfully demonstrate that the photochemical reactor and photochemical reaction method provided by this disclosure can effectively solve the core problems pointed out in the background art and fully achieve the expected inventive purpose and beneficial effects.

[0083] The above description is merely a preferred embodiment of this disclosure and an explanation of the technical principles employed. Those skilled in the art should understand that the scope of this disclosure is not limited to technical solutions formed by specific combinations of the above-described technical features, but should also cover other technical solutions formed by arbitrary combinations of the above-described technical features or their equivalents without departing from the above-described concept. For example, technical solutions formed by substituting the above features with (but not limited to) technical features disclosed in this disclosure that have similar functions.

[0084] Furthermore, while the operations are described in a specific order, this should not be construed as requiring these operations to be performed in the specific order shown or in a sequential order. In certain environments, multitasking and parallel processing may be advantageous. Similarly, while several specific implementation details are included in the above discussion, these should not be construed as limiting the scope of this disclosure. Certain features described in the context of individual embodiments may also be implemented in combination in a single embodiment. Conversely, various features described in the context of a single embodiment may also be implemented individually or in any suitable sub-combination in multiple embodiments.

[0085] Although the subject matter has been described using language specific to structural features and / or methodological logic, it should be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or actions described above. Rather, the specific features and actions described above are merely illustrative examples of implementing the claims.

[0086] The above description is merely a specific embodiment of this disclosure, enabling those skilled in the art to understand or implement it. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of this disclosure. Therefore, this disclosure is not to be limited to the embodiments described herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A photochemical reactor, characterized in that, include: A modular assembly box, wherein a slide rail is provided inside the modular assembly box, and the slide rail extends along a first direction; The multiple photochemical reaction modules located within the module assembly box are arranged along the first direction and are movable along the slide rail. The multiple photochemical reaction modules are used to sequentially absorb photons emitted by the light source to carry out photochemical reactions, wherein the first direction is parallel to the direction of the light emitted by the light source.

2. The photochemical reactor according to claim 1, characterized in that, The photochemical reaction module includes a reflux condenser, a condensate device, and a photochemical reaction tank; The photochemical reaction tank is used to contain the photoreaction liquid for carrying out the photochemical reaction; The condensate device is attached to and covers part of the outer wall of the photochemical reaction tank, and the condensate device is used to control the temperature inside the photochemical reaction tank; The reflux condenser is connected in series with the photochemical reaction cell, and the reflux condenser is used to condense and reflux volatile solvents.

3. The photochemical reactor according to claim 2, characterized in that, The photochemical reaction cell has a flat, hollow, three-dimensional structure, and its largest plane is perpendicular to the light emitted by the light source. One end of the photochemical reaction cell is provided with a connection port, and the reflux condenser is connected to the photochemical reaction cell through the connection port; The photochemical reaction cell is equipped with a sampling port at its edge.

4. The photochemical reactor according to claim 3, characterized in that, The photochemical reaction cell is equipped with a gas guide plate, which is densely covered with gas guide holes. The photochemical reaction cell has an air inlet at the end furthest from the connection port.

5. The photochemical reactor according to claim 3, characterized in that, The photochemical reaction cell is made of a highly transparent material, and its thickness along the first direction is 1-10 cm.

6. The photochemical reactor according to claim 2, characterized in that, The condensate device has a concave hollow three-dimensional structure. Along the first direction, the condensate device does not overlap with the photochemical reaction cell, and part of the condensate device is located between the reflux condensate device and the photochemical reaction cell. The condensate device has an outlet on the side near the reflux condenser and an inlet on the side away from the reflux condenser.

7. The photochemical reactor according to claim 6, characterized in that, The outer side of the condensate device is provided with a slider that matches the slide rail.

8. The photochemical reactor according to claim 3, characterized in that, The condensate device is located between the reflux condensate device and the photochemical reaction tank. The condensate device includes a first hole, and the connection port is located inside the first hole. The reflux condenser has an outlet on the side away from the connection port.

9. The photochemical reactor according to claim 1, characterized in that, The module assembly housing also includes a drive mechanism, which is used to drive the plurality of photochemical reaction modules to move along the slide rail.

10. A photochemical reaction method, characterized in that, The photochemical reactor used in any one of claims 1-9, wherein the photochemical reaction method comprises: Multiple photochemical reaction modules containing photoreaction liquids are placed inside the module assembly box; When the light source is turned on, the photons emitted by the light source sequentially initiate the photochemical reactions of each of the chemical reaction modules; After the photochemical reaction is completed in the photochemical reaction module that is closest to the light source, it is removed from the module assembly box; Move the other photochemical reaction modules inside the module assembly box toward the direction of the light source; A photochemical reaction module containing a photoreaction liquid is added to the side of the module assembly box away from the light source.

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