Photochemical reaction equipment
By adjusting the parameters of the light source system and the photoreaction vessel, the photochemical reaction equipment was optimized, solving the problems of spectral mismatch and unstable light intensity in traditional equipment. This enabled efficient and flexible control of photochemical reaction parameters, improving the yield and selectivity of the photoreaction.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
- Filing Date
- 2025-05-13
- Publication Date
- 2026-04-28
AI Technical Summary
Traditional photochemical reaction equipment is difficult to meet the precision and efficiency requirements of photochemical reaction parameter control in scientific research and production. Mismatched light source spectrum, poor light intensity stability, and unsuitable light spot shape and area lead to many side reactions, low photochemical reaction efficiency, and product yield and purity deviating from theoretical values.
A photochemical reaction device is provided, including a light source system, a photoreaction container, and a control system. The device can adjust parameters such as the wavelength, light intensity, light spot size and shape of the target light source, as well as the temperature, gas flow rate and photoreaction liquid flow rate of the photoreaction container. The photochemical reaction parameters are optimized through a beam shaping module and a light spot homogenizer.
It improves photon utilization, achieves high yield and high selectivity in synthesizing target products, shortens reaction time, and is applicable to various types of photochemical reactions, offering flexibility and versatility.
Smart Images

Figure CN224167501U_ABST
Abstract
Description
Technical Field
[0001] This disclosure relates to the field of photochemical reaction technology, and more particularly to a photochemical reaction device. Background Technology
[0002] In the field of photochemistry, precise control of photochemical reaction parameters is a core element in improving the yield and quality of target products. In recent years, with the deepening of scientific research and the continuous increase in production demands, increasingly higher requirements have been placed on the precision and efficiency of photochemical reaction conditions. Traditional photochemical reaction equipment has many limitations and cannot meet the growing needs of scientific research and production.
[0003] Firstly, traditional light sources are mainly mercury lamps and xenon lamps. Mercury lamps have spectra concentrated in a few discrete regions, lacking many spectral bands required for photochemical reactions, and they struggle to meet reaction conditions in complex photochemical reactions involving multiple wavelengths. Xenon lamps have broad and continuous spectra, but their light intensity fluctuates drastically across the entire spectrum; a precise wavelength with narrow linewidth across the entire wavelength range cannot be simultaneously achieved with high power intensity, making it difficult to meet the need for precise optimization of photochemical reaction parameters. In recent years, emerging LED light sources have limited commercial applications due to material and technological limitations in the ultraviolet region below 350 nanometers, resulting in insufficient output power and stability.
[0004] Secondly, traditional light sources adjust the output spectrum to a specific value by using gratings, filters, and filter solutions, resulting in a wide full-width spectrum. In photochemical reactions, the reactive bond energy is typically matched to the energy of a specific narrow-linewidth wavelength. The wide full-width of the emission spectrum from traditional light sources leads to numerous side reactions, low photoreaction efficiency, and a significant deviation of the yield and purity of the target product from theoretical values.
[0005] Furthermore, traditional light sources achieve light intensity regulation by changing the power supply voltage, resulting in low adjustment precision, poor light intensity stability, and short light source lifespan. This leads to numerous negative effects such as unstable photoreaction rate, low photon utilization, and uncertain product selectivity.
[0006] Furthermore, traditional light sources have fixed output spot shapes and areas, resulting in low adaptability to photoreaction containers. Photoreaction containers with larger spot areas have increased dead volumes, while those with smaller spot areas have low light energy utilization. The shape and area of the light spot affect the distribution of light energy in the reaction system, thereby affecting the uniformity and rate of the reaction.
[0007] Currently, scientific research and applications are expanding in depth in both microscopic and macroscopic directions. The control of photochemical reaction parameters in many fields, such as nanomaterial synthesis, solar energy conversion, and drug synthesis, is becoming increasingly refined. Developing a photochemical reaction device that can screen for better photochemical reaction parameters, improve photon utilization, and achieve high yield and high selectivity in the synthesis of target products has become a key issue that urgently needs to be solved in the field of photochemistry. It is of great significance for promoting related scientific research progress and industrial upgrading. Utility Model Content
[0008] To address the aforementioned technical problems, this disclosure provides a photochemical reaction apparatus that can screen for optimal photochemical reaction parameters, improve photon utilization, and achieve the goal of synthesizing target products with high yield and high selectivity.
[0009] In a first aspect, this disclosure provides a photochemical reaction apparatus, comprising: a light source system for providing a target light source required for the photochemical reaction, wherein the spectral range of the target light source includes the ultraviolet region, the visible region, and the infrared region; a photoreaction container for containing a photoreaction liquid to be subjected to the photochemical reaction; and a control system electrically connected to the light source system and the photoreaction container, wherein the control system controls the light source system to adjust a first parameter of the target light source, the first parameter including one or more of wavelength, light intensity, light spot size, light spot shape, and irradiation direction, and the control system is further used to control the photoreaction container to adjust a second parameter for the photochemical reaction, the second parameter including at least one or more of temperature, gas flow rate, and photoreaction liquid flow rate.
[0010] In some embodiments, the light source system includes a light source component and a beam shaping module; the light source component is used to adjust the wavelength and light intensity of the target light source; the beam shaping module is used to homogenize the light intensity of the target light source, adjust the spot size and spot shape of the target light source, and adjust the beam propagation direction of the target light source.
[0011] In some embodiments, the light source assembly includes a fundamental frequency light source, an optical mirror, an optical lens, and an optical frequency conversion crystal. The fundamental frequency light source is used to emit a light source in a first spectral range. The light beam emitted by the fundamental frequency light source is partially reflected by the optical lens and then directed to the optical mirror. After being reflected by the optical mirror, it is converted into a light source in a second spectral range by the optical frequency conversion crystal. The first spectral range and the second spectral range do not overlap.
[0012] In some embodiments, the beam shaping module includes a beam homogenizer, a beam shape and size adjuster, and a beam direction adjuster. The beam homogenizer is used to homogenize the light intensity of the target light source, the beam shape and size adjuster is used to adjust the beam size and shape of the target light source, and the beam direction adjuster is used to adjust the beam propagation direction of the target light source.
[0013] In some embodiments, the beam homogenizer includes one or more of the following: a microlens array, a molecular sieve, a soft-edge aperture, a phase-correcting and shaping lens group, and a square optical fiber.
[0014] In some embodiments, the spot shape and size adjuster includes one or more of the following: a beam expanding collimating lens group, a cylindrical lens, a square aperture, and a phase-correcting shaping lens group.
[0015] In some embodiments, the beam direction adjuster includes one or more of a beam deflection unit, an optical fiber collimating lens group, and an optical fiber.
[0016] In some embodiments, the photoreaction container includes a photoreaction container body and a condensation component. The condensation component is a cavity structure including a groove that matches the shape of the photoreaction container body. The cavity of the condensation component is used to contain condensate. The photoreaction container body is embedded in the groove and is used to contain the photoreaction liquid.
[0017] In some embodiments, the photoreaction container includes a non-flowing photoreaction container and a flowing photoreaction container, wherein the non-flowing photoreaction container is used for photochemical reactions with a defined volume of photoreaction liquid, and the flowing photoreaction container is used for photochemical reactions with an open volume of photoreaction liquid.
[0018] In some embodiments, the non-flowing photoreactor includes a photoreactor cavity as its main body, which has a flat, hollow, three-dimensional structure. The non-flowing photoreactor also includes a first inlet, a first outlet, and a first air inlet communicating with the photoreactor cavity, as well as a sand plate located within the photoreactor cavity. In the flowing photoreactor, the main body has a coiled structure, including a coiled microchannel. The two ports of the coiled microchannel are a second inlet and a second outlet, respectively. The flowing photoreactor also includes a raw material storage bottle, a product collection bottle, and a pump. The raw material storage bottle is connected to the second inlet via the pump, and the product collection bottle is connected to the second outlet. A gas guide tube is provided in the raw material storage bottle. The photoreactor also includes a condensate inlet and a condensate outlet communicating with a condensation component.
[0019] The technical solution provided in this disclosure has the following advantages compared with the prior art:
[0020] The photochemical reaction apparatus provided in this disclosure can adjust and optimize the first parameter of the target light source and the second parameter of the photochemical reaction, thereby screening for superior photochemical reaction parameters. This improves photon utilization, achieving high-yield and highly selective synthesis of the target product. Furthermore, it can increase quantum yield, shorten reaction time, and maximize the yield of photoreaction products, while also exhibiting high efficiency. Moreover, the photochemical reaction apparatus can flexibly adjust various parameters of the photochemical reaction according to different photochemical reaction requirements, making it suitable for various types of photochemical reactions and demonstrating flexibility and versatility. Attached Figure Description
[0021] 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.
[0022] 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.
[0023] Figure 1 This is a schematic diagram of the structure of a photochemical reaction device provided in this disclosure;
[0024] Figure 2 This is a schematic diagram of the structure of a light source assembly provided in this disclosure;
[0025] Figure 3 This is a schematic diagram of the structure of a photoreaction container provided in this disclosure.
[0026] Reference numerals: 10, Light source system; 11, Light source component; 111, Fundamental frequency light source; 112, Optical mirror; 113, Optical lens; 114, Optical frequency conversion crystal; 12, Beam shaping module; 20, Photoreaction container; 20a, Non-flowing photoreaction container; 20b, Flowing photoreaction container; 21, Photoreaction container body; 21a, Photoreaction container cavity; 21b, Coil microchannel; 211, First sample inlet; 212, First sample outlet; 213, First air inlet; 214, Sand plate; 215, Second sample inlet; 216, Second sample outlet; 217, Raw material storage bottle; 218, Product collection bottle; 219, Infusion pump; 2110, Gas guide tube; 22, Condensation component; 221, Condensate inlet; 222, Condensate outlet; 30, Control system. Detailed Implementation
[0027] 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.
[0028] 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.
[0029] 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 reaction apparatus, which includes:
[0030] The light source system 10 is used to provide the target light source required for the photochemical reaction, and the spectral range of the target light source includes the ultraviolet light region, the visible light region and the infrared light region;
[0031] Photoreaction container 20, which is used to contain the photoreaction liquid to be carried out in the photochemical reaction;
[0032] The control system 30 is electrically connected to the light source system 10 and the photoreaction container 20. The control system 30 is used to control the light source system 10 to adjust the first parameter of the target light source. The first parameter includes one or more of wavelength, light intensity, light spot size, light spot shape and irradiation direction. The control system 30 is also used to control the photoreaction container 20 to adjust the second parameter for the photochemical reaction. The second parameter includes at least one or more of temperature, gas flow rate and photoreaction liquid flow rate.
[0033] Specifically, this disclosure provides a photochemical reaction apparatus, which includes a light source system 10, a photoreaction container 20, and a control system 30. The light source system 10 provides the target light source required for the photochemical reaction; that is, the light source system 10 provides the light energy required for the photochemical reaction to the photoreaction container 20. The light source system 10 is located outside the photoreaction container 20 and is an external light source. The light source provided by the light source system 10 enters the photoreaction liquid vertically from the side, top, or bottom of the photoreaction container 20. The photoreaction container 20 is used to contain the photoreaction liquid to be subjected to the photochemical reaction; that is, the photoreaction container 20 can be used to contain the photoreaction liquid and provide a place for the photochemical reaction to take place.
[0034] The target light source provided by the light source system 10 has a spectral range including the ultraviolet, visible, and infrared regions, covering a wide range of photochemical reactions. In some optional embodiments, the target light source provided by the light source system 10 has a spectral range of 230-1080 nanometers, including the ultraviolet (230-400 nanometers), visible (400-760 nanometers), and infrared (760-1080 nanometers) regions, covering a wide range of photochemical reactions.
[0035] The control system 30 is electrically connected to the light source system 10 and the photoreaction container 20. The control system 30 is used to control the light source system 10 to adjust the first parameters of the target light source. The first parameters include one or more of wavelength, light intensity, light spot size, light spot shape, and irradiation direction. That is, the control system 30 can be used to set the first parameters of the target light source and control the light source system 10 to adjust these parameters. The control system 30 is also used to control the photoreaction container 20 to adjust the second parameters for the photochemical reaction. The second parameters include at least one or more of temperature, gas flow rate, and photoreaction liquid flow rate. That is, the control system 30 can be used to set the second parameters for the photochemical reaction and control the photoreaction container 20 to adjust these parameters. In other words, for a specific photochemical reaction, the photochemical reaction equipment can adjust and optimize the first parameters of the target light source and the second parameters for the photochemical reaction, i.e., screen for better photochemical reaction parameters, thereby improving photon utilization and achieving high-yield, high-selectivity synthesis of the target product. It can also improve quantum yield, shorten reaction time, maximize the yield of the photoreaction product, and simultaneously achieve high efficiency. Meanwhile, the photochemical reaction equipment can flexibly adjust various parameters of the photochemical reaction according to different photochemical reaction requirements, and is suitable for a variety of types of photochemical reactions, with flexibility and versatility.
[0036] When conducting photochemical experiments using the photochemical reaction device provided in this embodiment, a photoreaction solution can be prepared first, transferred to the photoreaction container 20, and then, based on the absorption spectrum of the photoreaction solution, the first parameter of the target light source can be adjusted by the control system 30 controlling the light source system 10, and the second parameter for the photochemical reaction can be adjusted by the control system 30 controlling the photoreaction container 20. Then, the light source system 10 can be started to carry out the photochemical reaction.
[0037] In some optional embodiments, when using the photochemical reaction device provided in this embodiment to conduct photochemical experiments, the light intensity of the target light source can be adjusted to a fixed intensity by the control system 30 to control the light source system 10 according to the absorption spectrum of the photoreaction liquid. The wavelength of the target light source can be adjusted to multiple different test wavelengths by the control system 30 to control the light source system 10 in sequence. The light source system 10 is started in sequence to carry out photochemical reactions, and the yield of the target product and the selectivity of the photochemical reaction are measured in sequence.
[0038] That is, based on the absorption spectrum of the photoreaction liquid, the light intensity of the target light source is adjusted to a fixed light intensity W0 by the light source system 10 controlled by the control system 30. The wavelengths of the target light source are set to λ1, λ2, λ3, λ4, etc. according to the ultraviolet-visible absorption spectrum of the photoreaction liquid. The process of the above photochemical reaction method is repeated to complete the photochemical reaction under each wavelength. The yield of the target product is quantitatively detected in sequence, and the selectivity of the photochemical reaction is calculated.
[0039] Then, the dependence of the target product yield and selectivity on the wavelength of the target light source was established, and the optimal wavelength λ of the target light source for the photochemical reaction was determined. max .
[0040] The control system 30 controls the light source system 10 to adjust the wavelength of the target light source to the preferred wavelength. The control system 30 controls the light source system 10 to adjust the light intensity of the target light source to multiple different test light intensities in turn. The light source system 10 is started in turn to carry out photochemical reactions in turn. The yield of the target product is quantitatively detected in turn, and the selectivity of the photochemical reaction is calculated.
[0041] That is, the preferred wavelength λ of the fixed target light source max The light intensities of the target light source were set to W1, W2, W3, W4, etc., and the process of the above photochemical reaction method was repeated to complete the photochemical reaction under each wavelength. The yield of the target product and the selectivity of the photochemical reaction were then quantitatively detected and calculated.
[0042] Next, the dependence of the target product yield and selectivity on the light intensity of the target light source was established, and the optimal light intensity W of the target light source for the photochemical reaction was determined. max .
[0043] Next, the control system 30 controls the light source system 10 to adjust the wavelength of the target light source to the preferred wavelength, the control system 30 controls the light source system 10 to adjust the light intensity of the target light source to the preferred light intensity, and the control system 30 controls the photoreaction container 20 to adjust the second parameter for the photochemical reaction. The light source system 10 is started sequentially to carry out the photochemical reaction, and the yield of the target product and the selectivity of the photochemical reaction are quantitatively detected sequentially.
[0044] That is, at the preferred wavelength λ of the fixed target light source max And the preferred light intensity W of the fixed target light source max During the process, parameters such as temperature, reaction solution concentration, gas flow rate, and photoreaction solution flow rate are optimized for photochemical reactions, and the yield of the target product is quantitatively detected and the selectivity of the photochemical reaction is calculated in sequence.
[0045] Finally, the dependence of the target product yield and selectivity on the second parameter was established to determine the preferred second parameter for the photochemical reaction.
[0046] When using the photochemical reaction device provided in this embodiment to carry out photochemical reactions, the preferred wavelength of the target light source for the photochemical reaction can be accurately screened and determined, so that the target product of the reaction has a higher yield and higher selectivity. Furthermore, by optimizing the light intensity, light spot shape and size, the quantum yield of light can be effectively improved, the reaction time can be shortened, and the yield of photoreaction products can be maximized, while also being highly efficient.
[0047] Optionally, during the photochemical reaction, the process can be monitored in real time using thin-layer chromatography, high-performance liquid chromatography, gas chromatography, etc. High-performance liquid chromatography, 1H NMR, gas chromatography, etc., can be used to quantitatively detect the yield of the target product and calculate the selectivity of the photochemical reaction.
[0048] In some alternative embodiments, the control system 30 includes a parameter adjustment interface that can be used to adjust a first parameter of the target light source and a second parameter for the photochemical reaction. For example, the parameter adjustment interface may be a display screen.
[0049] In some alternative embodiments, the light source system 10 can be used to feed back the first parameter of the target light source to the control system 30, the photoreaction container 20 can be used to feed back the second parameter of the photochemical reaction to the control system 30, and the control system 30 can be used to monitor the operating status of the photochemical reaction device in real time.
[0050] In some alternative embodiments, the control system 30 also includes an alarm module that can be used to issue a fault alarm when a problem occurs in the operation of the photochemical reaction equipment.
[0051] Continue to refer to Figure 1 In some alternative embodiments, the light source system 10 includes a light source assembly 11 and a beam shaping module 12;
[0052] The light source assembly 11 is used to adjust the wavelength and light intensity of the target light source;
[0053] The beam shaping module 12 is used to homogenize the light intensity of the target light source, adjust the spot size and shape of the target light source, and adjust the beam propagation direction of the target light source.
[0054] Specifically, the light source system 10 includes a light source component 11, which adjusts the wavelength and light intensity of the target light source. The light source system 10 also includes a beam shaping module 12, which optimizes the light intensity of the target light source, adjusts the spot size and shape of the target light source, and changes the beam propagation direction of the target light source.
[0055] Specifically, the wavelength of the target light source can be adjusted by setting the light source component 11, and can be adjusted to the preferred wavelength, so that the target product of the reaction has a higher yield and higher selectivity. Furthermore, the light intensity, spot size, spot shape and propagation direction of the target light source can be adjusted by setting the light source component 11 and the beam shaping module 12, and each parameter is adjusted to the optimal value, which effectively improves the photon yield, shortens the reaction time, maximizes the yield of photoreaction products, and is also highly efficient.
[0056] Figure 2 This is a schematic diagram of the structure of a light source assembly provided in this disclosure, for reference. Figure 1 and Figure 2 In some optional embodiments, the light source assembly 11 includes a baseband light source 111, an optical mirror 112, an optical lens 113, and an optical frequency conversion crystal 114. The baseband light source 111 is used to emit a light source in a first spectral range. The light beam emitted by the baseband light source 111 is partially reflected by the optical lens 113 and then directed to the optical mirror 112. After being reflected by the optical mirror 112, it is converted into a light source in a second spectral range by the optical frequency conversion crystal 114. The first spectral range and the second spectral range do not overlap.
[0057] Specifically, the light source assembly 11 includes a fundamental frequency light source 111, an optical reflector 112, an optical lens 113, and an optical frequency conversion crystal 114. The fundamental frequency light source 111 is used to emit light within a first spectral range. The light beam emitted by the fundamental frequency light source 111 is partially directly emitted through the optical lens 113, thus the light source assembly 11 can emit a fundamental frequency light source within the first spectral range. Optionally, the fundamental frequency light source 111 can be a laser light source, which has strong monochromaticity and allows for precise tuning of the light wavelength and intensity. Optionally, the fundamental frequency light source 111 can be a Ti:sapphire fundamental frequency light source with an emission spectral range of 680-1080 nanometers. That is, the first spectral range can be 680-1080 nanometers. The light emitted by the fundamental frequency light source 111 is partially reflected by the optical lens 113 and then directed to the optical reflector 112. After being reflected by the optical reflector 112, it is converted into a frequency conversion light source within a second spectral range by the optical frequency conversion crystal 114. The first and second spectral ranges do not partially overlap. The second spectral range can be 230-680 nanometers. Thus, the target light source provided by the light source component 11 can have a spectral range of 230-1080 nanometers, including the ultraviolet region (230-400 nanometers), the visible region (400-760 nanometers), and the infrared region (760-1080 nanometers), which can cover a wide range of photochemical reactions.
[0058] Optionally, the target light source can be continuously tunable in the spectral range of 230-1080 nm, with a single wavelength half-width of ≤0.1 nm and a light intensity continuously tunable in the range of 0-100 mW.
[0059] In some alternative embodiments, the optical frequency conversion crystal 114 can be one or a combination of BBO, LBO, KTP, KDP, LCB, CBO, and NSBBF. The control system 30 can adjust the wavelength of the light source by controlling the temperature and angle of the optical frequency conversion crystal 114.
[0060] Continue to refer to Figure 1 The beam shaping module 12 includes a beam homogenizer (not shown in the figure), a beam shape and size adjuster (not shown in the figure), and a beam direction adjuster (not shown in the figure). The beam homogenizer is used to homogenize the light intensity of the target light source, the beam shape and size adjuster is used to adjust the beam size and shape of the target light source, and the beam direction adjuster is used to adjust the beam propagation direction of the target light source.
[0061] Specifically, the light source system 10 includes a beam shaping module 12, which comprises a beam homogenizer, a beam shape and size adjuster, and a beam direction adjuster. The beam homogenizer homogenizes the light intensity of the target light source, the beam shape and size adjuster adjusts the beam size and shape of the target light source, and the beam direction adjuster adjusts the propagation direction of the target light source. Thus, the beam shaping module 12 optimizes the light intensity of the target light source, adjusts the beam size and shape of the target light source, and changes the propagation direction of the light from the target light source.
[0062] In some optional embodiments, the beam homogenizer includes one or more of the following: a microlens array, a molecular sieve, a soft-edge aperture, an aberration-correcting lens group, and a square optical fiber. It can homogenize the Gaussian-distributed light intensity into a flat-top distribution, thereby homogenizing the light intensity of the target light source. Of course, in other embodiments of this disclosure, the beam homogenizer may also include other beam homogenizers, which will not be described in detail here.
[0063] In some optional embodiments, the spot shape and size adjuster includes one or more of the following: a beam expanding and collimating lens group, a cylindrical lens, a square aperture, and a phase-correcting and shaping lens group. This adjuster can modify the shape and size of the spot formed by the target light source, transforming a point-like spot into different sizes such as circles, squares, ellipses, and spindles, so that the shape and size of the spot formed by the target light source matches the photoreaction container. Of course, in other embodiments of this disclosure, the spot shape and size adjuster may also include other spot shape and size adjusters, which will not be described in detail here.
[0064] In some optional embodiments, the beam direction adjuster includes one or more of a beam deflection unit, an optical fiber collimating lens group, and an optical fiber, which can change the propagation direction of the beam emitted by the light source assembly to form top-illuminated, side-illuminated, and bottom-illuminated modes, thereby adjusting the propagation direction of the target light source so that the beam formed by the target light source can enter the interior of the photoreaction container perpendicularly.
[0065] Figure 3 This is a schematic diagram of the structure of a photoreactor provided in this disclosure, for reference. Figure 1 and Figure 3 In some optional embodiments, the photoreaction container 20 includes a photoreaction container body 21 and a condensation component 22. The condensation component 22 is a cavity structure including a groove that matches the shape of the photoreaction container body 21. The cavity of the condensation component 22 is used to contain condensate. The photoreaction container body 21 is embedded in the groove and is used to contain the photoreaction liquid.
[0066] Specifically, the photoreaction container 20 includes a photoreaction container body 21 and a condensation component 22. The photoreaction container body 21 is used to contain the photoreaction liquid. Optionally, the material of the photoreaction container body 21 can be highly transparent quartz glass. The condensation component 22 is a cavity structure including a groove that matches the shape of the photoreaction container body 21, so that the photoreaction container body 21 can be embedded in the groove of the condensation component 22, and the cavity of the condensation component 22 can be used to contain condensate for controlling the temperature of the photochemical reaction.
[0067] Continue to refer to Figure 1 and Figure 3 In some alternative embodiments, the photoreaction container 20 includes a non-flowing photoreaction container 20a and a flowing photoreaction container 20b.
[0068] Specifically, the photoreaction container 20 includes at least two types of photoreaction containers, namely a non-flowing photoreaction container 20a and a flowing photoreaction container 20b. Of course, in other embodiments of this disclosure, the photoreaction container 20 may also include other types of photoreaction containers, which will not be described in detail here.
[0069] The non-flowing photoreaction vessel 20a is suitable for photochemical reactions with a fixed volume of photoreaction liquid, while the flowing photoreaction vessel 20b is suitable for photochemical reactions with an open volume of photoreaction liquid, and can be applied to different photochemical reaction scenarios.
[0070] Continue to refer to Figure 1 and Figure 3 In some optional embodiments, the non-flowing photoreaction container 20a includes a photoreaction container cavity 21a in the main body 21 of the photoreaction container 21a. The structure of the photoreaction container cavity 21a is a flat, hollow three-dimensional structure. The non-flowing photoreaction container 20a also includes a first sample inlet 211, a first sample outlet 212 and a first air inlet 213 that are in communication with the photoreaction container cavity 21a, and a sand plate 214 located in the photoreaction container cavity 21a.
[0071] The main body 21 of the flowable photoreactor 20b has a coil-like structure. The main body 21 includes a coil microchannel 21b, and the two ports of the coil microchannel 21b are a second inlet 215 and a second outlet 216, respectively. The flowable photoreactor 20b also includes a raw material storage bottle 217, a product collection bottle 218 and a pump 219. The raw material storage bottle 217 is connected to the second inlet 215 through the pump 219, and the product collection bottle 218 is connected to the second outlet 216. A gas guide tube 2110 is provided in the raw material storage bottle 217.
[0072] The photo-reaction vessel 20 also includes an inlet 221 and an outlet 222 that communicate with the condenser 22.
[0073] Specifically, the non-flowing photoreaction container 20a includes a photoreaction container cavity 21a, which has a flat, hollow, three-dimensional structure. The non-flowing photoreaction container 20a also includes a first sample inlet 211, a first sample outlet 212, and a first air inlet 213 that communicate with the photoreaction container cavity 21a, as well as a sand plate 214 located inside the photoreaction container cavity 21a. The photoreaction liquid enters the photoreaction container cavity 21a through the first sample inlet 211, and the gas enters the photoreaction container cavity 21a through the first air inlet 213. A sand plate 214 is installed inside the photoreaction container cavity 21a, with the first sample inlet 211 and the first sample outlet 212 located on one side of the sand plate 214, and the first air inlet 213 located on the other side. During the photochemical reaction, stable bubbles can be formed using the sand plate 214 to agitate the photoreaction liquid, achieving mass and heat transfer and balancing the photochemical reaction. The target light source enters the photoreaction container cavity 21a perpendicularly to the side with the largest area of the non-flowing photoreaction container 20a. After the photoreaction liquid undergoes the photochemical reaction, it can be discharged through the first sample outlet 212. Therefore, the non-flowing photoreaction container 20a is suitable for photochemical reactions of a fixed volume of photoreaction liquid.
[0074] The main body 21 of the flow-through photoreactor 20b has a coiled structure, including a coiled microchannel 21b. Optionally, the coiled microchannel 21b can be a microchannel with an inner diameter of no more than 2 mm. The two ports of the coiled microchannel 21b are a second inlet 215 and a second outlet 216, respectively. The flow-through photoreactor 20b also includes a raw material storage bottle 217, a product collection bottle 218, and a pump 219. The raw material storage bottle 217 is connected to the second inlet 215 through the pump 219, and the product collection bottle 218 is connected to the second outlet 216. A gas guide tube 2110 is provided in the raw material storage bottle 217. The volume of the photoreaction liquid in the flow-type photoreaction container 20b is not fixed. The photoreaction liquid is stored in the raw material storage bottle 217. Gas enters the raw material storage bottle 217 through the gas guide tube 2110. The infusion pump 219 pushes the photoreaction liquid from the raw material storage bottle 217 continuously into the coil microchannel 21b through the second sample inlet 215 at a certain speed. During the flow, the photoreaction liquid is automatically disturbed and mixed. The target light source enters the coil microchannel 21b perpendicular to the plane of the non-flow-type photoreaction container 20a. After the photoreaction liquid undergoes a photochemical reaction, it flows out from the second sample outlet 216 and enters the product collection bottle 218. Thus, the flow-type photoreaction container 20b is suitable for photochemical reactions with open-volume photoreaction liquid and can be applied to different photochemical reaction scenarios.
[0075] The photochemical reaction vessel 20 also includes an inlet 221 and an outlet 222 that communicate with the condenser 22. The condensate enters the condenser 22 through the condensate inlet 221 and exits the condenser 22 through the condensate outlet 222. The temperature of the photochemical reaction is controlled by controlling the flow rate of the condensate.
[0076] When performing a photochemical reaction using the photochemical device provided in this embodiment, since the photoreaction container 20 includes a non-flowing photoreaction container 20a and a flowing photoreaction container 20b, either the non-flowing photoreaction container 20a or the flowing photoreaction container 20b is selected as the photoreaction container before the photochemical reaction begins. When the non-flowing photoreaction container 20a is selected as the photoreaction container, gas is first introduced into the main body 21 of the photoreaction container. Then, the photoreaction liquid is transferred into the main body 21 of the photoreaction container. The circulation of the condensate in the condensation component 22 is started, and the temperature of the photochemical reaction is monitored by the control system 30. The gas flow rate for the photochemical reaction is also adjusted by the control system 30.
[0077] When selecting a flowable photoreaction vessel 20b as the photoreaction vessel for the photochemical reaction, the photoreaction liquid is first transferred to the raw material storage bottle 217, and then the gas participating in the photochemical reaction is introduced into the raw material storage bottle 217. The circulation of the condensate in the condensation component 22 is started, and the temperature of the photochemical reaction is monitored by the control system 30. The infusion pump 219 is started to continuously input the photoreaction liquid into the main body 21 of the photoreaction vessel. After photoreaction, it enters the product collection bottle 218. The flow rate of the gas and the flow rate of the photoreaction liquid are adjusted by the control system 30.
[0078] Exemplary, this embodiment provides a specific example of using the above-described photochemical reaction equipment to precisely optimize the parameters of the photochemical reaction for the production of pre-vitamin D2 from ergosterol:
[0079] At room temperature (25°C), 2.4 g of ergosterol was dissolved in 500 mL of a mixed solvent of methanol and n-hexane (methanol:n-hexane = 3:1) to prepare a photoreaction solution.
[0080] The control system was activated, a non-flowing photoreactor was configured, and a side-illumination mode was set. The nitrogen flow rate was set to 1 L / min, the condenser temperature to 20°C, the target light source wavelength to 273 nm, the light intensity to 220 mW, and the spot size to a 5 × 6 cm² rectangle. The nitrogen gas and condenser were turned on, and 20 mL of the photoreaction solution was transferred to the non-flowing photoreactor. The light source system was activated, and the photochemical reaction was stopped after 30 minutes of illumination. The product distribution under these reaction conditions was determined using high-performance liquid chromatography (HPLC): ergosterol 90.2%, pre-vitamin D2 9.1%, rapestrol 0.6%, and vitamin D2 0.1%.
[0081] In the above operation, the wavelength of the target light source was switched to 282 nm, while other conditions remained unchanged. After 30 minutes of photochemical irradiation, the photochemical reaction was terminated. High-performance liquid chromatography (HPLC) was used to analyze the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 66.7%, previtamin D2 27.2%, paclitaxel 5.9%, photosterol 0.1%, and vitamin D2 0.1%.
[0082] In the above operation, the wavelength of the target light source was switched to 289 nm, while other conditions remained unchanged. After 30 minutes of photochemical irradiation, the photochemical reaction was terminated. High-performance liquid chromatography (HPLC) was used to analyze the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 19.2%, previtamin D2 55.6%, paclitaxel 23.9%, photosterol 1.1%, and vitamin D2 0.2%.
[0083] In the above operation, the wavelength of the target light source was switched to 300 nm, while other conditions remained unchanged. After 30 minutes of photochemical irradiation, the photochemical reaction was terminated. High-performance liquid chromatography (HPLC) was used to analyze the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 4.9%, previtamin D2 71.6%, paclitaxel 20.6%, photosterol 2.8%, and vitamin D2 0.1%.
[0084] In the above operation, the wavelength of the target light source was switched to 304 nm, while other conditions remained unchanged. After 30 minutes of photochemical irradiation, the photochemical reaction was terminated. High-performance liquid chromatography (HPLC) was used to analyze the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 14.6%, previtamin D2 61.4%, paclitaxel 17.5%, photosterol 6.2%, and vitamin D2 0.2%.
[0085] In the above operation, the wavelength of the target light source was switched to 300 nm, the light intensity was adjusted to 100 mW, and other conditions remained unchanged. After 20 minutes of photochemical reaction, the photochemical reaction was terminated. The product distribution under these reaction conditions was determined by high-performance liquid chromatography (HPLC) analysis of the photoreaction solution: ergosterol 68.3%, previtamin D2 28.5%, and tachysterol 3.2%.
[0086] In the above operation, the wavelength of the target light source was fixed at 300 nm, the light intensity was adjusted to 135 mW, and other conditions remained unchanged. After 20 minutes of photochemical reaction, the photochemical reaction was terminated. The product distribution under these reaction conditions was determined by high-performance liquid chromatography (HPLC) analysis of the photoreaction solution: ergosterol 49.6%, previtamin D2 44.7%, rapestrol 5.6%, and photosterol 0.2%.
[0087] In the above operation, the wavelength of the target light source was fixed at 300 nm, the light intensity was adjusted to 182 mW, and other conditions remained unchanged. After 20 minutes of photocatalytic reaction, the photochemical reaction was terminated. High-performance liquid chromatography (HPLC) was used to analyze the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 37.5%, previtamin D2 53.2%, rapestrol 8.5%, photosterol 0.7%, and vitamin D2 0.1%.
[0088] In the above operation, the wavelength of the target light source was fixed at 300 nm, the light intensity was adjusted to 227 mW, and other conditions remained unchanged. After 20 minutes of photochemical irradiation, the photochemical reaction was terminated. High-performance liquid chromatography (HPLC) was used to analyze the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 24.6%, previtamin D2 61.8%, paclitaxel 12.1%, photosterol 1.4%, and vitamin D2 0.1%.
[0089] In the above operation, the wavelength of the target light source was fixed at 300 nm, the light intensity was adjusted to 285 mW, and other conditions remained unchanged. After 20 minutes of photocatalytic reaction, the photochemical reaction was terminated. High-performance liquid chromatography (HPLC) was used to analyze the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 0.9%, previtamin D2 78.5%, paclitaxel 18.6%, photosterol 1.9%, and vitamin D2 0.1%.
[0090] Based on the above data, the parameters of the photochemical reaction for the production of pre-vitamin D2 from ergosterol can be precisely optimized.
[0091] It should be noted that this embodiment only illustrates an example of precisely optimizing the parameters of the photochemical reaction for the generation of pre-vitamin D2 from ergosterol using the above-described photochemical reaction equipment. In other embodiments of this disclosure, other photochemical reactions can also be achieved using the above-described photochemical reaction equipment, and this disclosure does not make specific limitations here.
[0092] The photochemical reaction equipment provided in this embodiment can accurately screen and determine the preferred wavelength of the target light source for the photochemical reaction, resulting in higher yields and selectivity of the target products. Furthermore, by optimizing light intensity, spot shape, and size, the equipment effectively improves quantum yield, shortens reaction time, and maximizes the yield of photoreaction products while maintaining high efficiency. In addition, the equipment can flexibly adjust various parameters of the photochemical reaction according to different reaction requirements, making it suitable for various types of photochemical reactions and demonstrating flexibility and versatility.
[0093] 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.
[0094] 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.
[0095] 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.
[0096] 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 reaction apparatus, characterized in that, include: A light source system, wherein the light source system is used to provide the target light source required for the photochemical reaction, and the spectral range of the target light source includes the ultraviolet light region, the visible light region, and the infrared light region; A photoreaction container, wherein the photoreaction container is used to contain a photoreaction liquid to be subjected to a photochemical reaction; The control system is electrically connected to the light source system and the photoreaction container. The control system is used to control the light source system to adjust a first parameter of the target light source. The first parameter includes one or more of wavelength, light intensity, light spot size, light spot shape, and irradiation direction. The control system is also used to control the photoreaction container to adjust a second parameter for the photochemical reaction. The second parameter includes at least one or more of temperature, gas flow rate, and photoreaction liquid flow rate.
2. The photochemical reaction apparatus according to claim 1, characterized in that, The light source system includes a light source component and a beam shaping module; The light source component is used to adjust the wavelength and light intensity of the target light source; The beam shaping module is used to homogenize the light intensity of the target light source, adjust the spot size and shape of the target light source, and adjust the beam propagation direction of the target light source.
3. The photochemical reaction apparatus according to claim 2, characterized in that, The light source assembly includes a base frequency light source, an optical mirror, an optical lens, and an optical frequency conversion crystal. The base frequency light source is used to emit light in a first spectral range. The light beam emitted by the base frequency light source is partially reflected by the optical lens and then directed to the optical mirror. After being reflected by the optical mirror, it is converted into light in a second spectral range by the optical frequency conversion crystal. The first spectral range and the second spectral range do not overlap.
4. The photochemical reaction apparatus according to claim 3, characterized in that, The beam shaping module includes a beam homogenizer, a beam shape and size adjuster, and a beam direction adjuster. The beam homogenizer is used to homogenize the light intensity of the target light source, the beam shape and size adjuster is used to adjust the beam size and shape of the target light source, and the beam direction adjuster is used to adjust the beam propagation direction of the target light source.
5. The photochemical reaction apparatus according to claim 4, characterized in that, The light spot homogenizer includes one or more of the following: microlens array, molecular sieve, soft-edge aperture, phase-correcting and shaping lens group, and square optical fiber.
6. The photochemical reaction apparatus according to claim 4, characterized in that, The light spot shape and size adjuster includes one or more of the following: a beam expanding collimating lens group, a cylindrical lens, a square aperture, and a phase-correcting and shaping lens group.
7. The photochemical reaction apparatus according to claim 4, characterized in that, The beam direction adjuster includes one or more of the following: a beam deflection unit, an optical fiber collimating lens group, and an optical fiber.
8. The photochemical reaction apparatus according to claim 1, characterized in that, The photoreaction container includes a photoreaction container body and a condensation component. The condensation component is a cavity structure with a groove that matches the shape of the photoreaction container body. The cavity of the condensation component is used to contain condensate. The photoreaction container body is embedded in the groove and is used to contain the photoreaction liquid.
9. The photochemical reaction apparatus according to claim 8, characterized in that, The photoreaction container includes a non-flowing photoreaction container and a flowing photoreaction container. The non-flowing photoreaction container is used for photochemical reactions with a defined volume of photoreaction liquid, while the flowing photoreaction container is used for photochemical reactions with an open volume of photoreaction liquid.
10. The photochemical reaction apparatus according to claim 9, characterized in that, The non-flowing photoreaction container includes a photoreaction container cavity, which has a flat, hollow, three-dimensional structure. The non-flowing photoreaction container also includes a first sample inlet, a first sample outlet, and a first air inlet that communicate with the photoreaction container cavity, as well as a sand plate located inside the photoreaction container cavity. The photoreaction container includes a flow-through photoreaction container. The main body of the flow-through photoreaction container has a coil-like structure. The main body of the photoreaction container includes a coil microchannel. The two ports of the coil microchannel are a second inlet and a second outlet, respectively. The flow-through photoreaction container also includes a raw material storage bottle, a product collection bottle, and a pump. The raw material storage bottle is connected to the second inlet through the pump. The product collection bottle is connected to the second outlet. A gas guide tube is provided in the raw material storage bottle. The photoreaction container also includes a condensate inlet and a condensate outlet that communicate with the condensation component.