Photochemical reaction equipment and photochemical reaction method
By introducing adjustable light source and reaction vessel parameters into the photochemical reaction equipment, the problem that traditional equipment is difficult to accurately regulate the photochemical reaction parameters is solved, and efficient and selective photochemical reactions are achieved.
Patent Information
- Application Number
- CN202510613883.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-13
- Publication Date
- 2025-06-24
AI Technical Summary
Traditional photochemical reaction equipment is difficult to accurately regulate the photochemical reaction parameters, resulting in low photoreaction efficiency and deviation from the theoretical value of product yield and purity.
A photochemical reaction device is provided, including a light source system, a photoreaction vessel and a control system, capable of adjusting the wavelength, light intensity, spot size, shape and irradiation direction of the target light source, as well as the temperature, gas flow rate and photoreaction liquid flow rate of the photoreaction vessel.
By optimizing photochemical reaction parameters, the photon utilization rate is improved, the target product is synthesized with high yield and high selectivity, the photoquantum yield is improved, and the reaction time is shortened.
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Figure CN120189894A_ABST
Abstract
Description
Technical Field
[0001] The present disclosure relates to the technical field of photochemical reaction, and in particular to a photochemical reaction device and a photochemical reaction method. Background Art
[0002] In the field of photochemistry, precisely regulating photochemical reaction parameters is the core element for improving the yield and quality of target products. In recent years, with the continuous deepening of scientific research and the continuous increase in production demand, higher requirements have been put forward for the precision and efficiency of photochemical reaction conditions. Traditional photochemical reaction devices have many limitations and are difficult to meet the growing scientific research and production needs.
[0003] First of all, traditional light sources are mainly mercury lamps and xenon lamps. The spectrum of mercury lamps is concentrated in several discrete regions, lacking many spectral bands required for photochemical reactions, and it is difficult to meet the reaction conditions in complex photochemical reactions with multi-wavelength cooperation; xenon lamps have a broad and continuous spectrum, but the light intensity fluctuates violently throughout the spectrum, and it is impossible to have both precise light wavelengths with narrow line widths in the whole band and high-power light intensity, making it difficult to meet the requirements for precisely optimizing photochemical reaction parameters. In recent years, the emerging LED light sources have limited output power and stability in the ultraviolet region below 350 nanometers due to material and technology limitations, and their commercial applications are limited.
[0004] Secondly, traditional light sources adjust the output of specific spectra by means of loading gratings, filters, filter liquids, etc., and the full width at half maximum of the spectrum is large. In photochemical reactions, the reaction active bond energy usually matches the energy of specific narrow-line-width light wavelengths. The large full width at half maximum of the emission spectrum of traditional light sources leads to many side reactions, low photochemical reaction efficiency, and a large deviation of the yield and purity of target products from the theoretical values.
[0005] Thirdly, traditional light sources adjust the light intensity of the light source by changing the power supply voltage, with low adjustment accuracy, poor light intensity stability, and short light source life, resulting in many negative effects such as unstable photochemical reaction rates, low photon utilization rates, and uncertain product selectivity.
[0006] In addition, the shape and area of the output light spot of traditional light sources are fixed, with low adaptability to photochemical reaction vessels. The dead volume of photochemical reaction vessels larger than the light spot area increases, and the light energy utilization rate of photochemical reaction vessels smaller than the light spot area is low. The shape and area of the light spot affect the distribution of light energy in the reaction system, thereby affecting the uniformity and reaction rate of the reaction.
[0007] At present, scientific research and application are expanding in depth in both micro and macro directions. The regulation of photochemical reaction parameters in many fields such as nanomaterial synthesis, solar energy conversion, and drug synthesis is becoming more and more sophisticated. The development of a photochemical reaction equipment that can screen better photochemical reaction parameters, improve photon utilization, and achieve high-yield and high-selectivity synthesis of target products has become a key issue that needs to be urgently solved in the field of photochemistry, and is of great significance to promoting related scientific research progress and industrial upgrading. Summary of the invention
[0008] In order to solve the above technical problems, the present disclosure provides a photochemical reaction device and a photochemical reaction method, which can screen better photochemical reaction parameters, improve photon utilization, and achieve the purpose of synthesizing target products with high yield and high selectivity.
[0009] In a first aspect, the present disclosure provides a photochemical reaction device, comprising: a light source system, the light source system is used to provide a 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, the photoreaction container is used to contain a photoreaction liquid to be subjected to a photochemical reaction; a control system, 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, spot size, spot shape and irradiation direction, and 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.
[0010] In some embodiments, the light source system includes a light source assembly and a beam shaping module; the light source assembly is used to adjust the wavelength and light intensity of the target light source, the light source assembly includes a fundamental frequency light source, an optical reflector, 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 emitted to the optical reflector, and after being reflected by the optical reflector, it is converted into a light source in a second spectral range by the optical frequency conversion crystal, and the first spectral range and the second spectral range do not overlap in part; the beam shaping module includes a spot homogenizer, a spot shape size regulator and a beam direction regulator, the spot homogenizer is used to homogenize the light intensity of the target light source, the spot shape size regulator is used to adjust the spot size and spot shape of the target light source, and the beam direction regulator is used to adjust the beam propagation direction of the target light source.
[0011] In some embodiments, the spot homogenizer includes one or more of a microlens array, a molecular sieve, a soft-edge aperture, an aberration shaping lens group, and a square optical fiber.
[0012] In some embodiments, the spot shape size adjuster includes one or more of a beam expansion collimating lens group, a cylindrical lens, a square aperture, and an aberration shaping lens group.
[0013] In some embodiments, the beam direction adjuster includes one or more of a beam turning unit, an optical fiber collimating lens group, and an optical fiber.
[0014] In some embodiments, the photoreaction vessel includes a photoreaction vessel body and a condensation component. The condensation component is a cavity structure including a groove that fits the shape of the photoreaction vessel body. The cavity of the condensation component is used to hold the condensate. The photoreaction vessel body is embedded in the groove, and the photoreaction vessel body is used to hold the photoreaction solution.
[0015] In some embodiments, the photoreaction vessel includes a non-flow photoreaction vessel and a flow photoreaction vessel; in the non-flow photoreaction vessel, the photoreaction vessel body includes a photoreaction vessel cavity, and the structure of the photoreaction vessel cavity is a flat and hollow three-dimensional structure. The non-flow photoreaction vessel further includes a first sample inlet, a first sample outlet, a first gas inlet that communicates with the photoreaction vessel cavity, and a sand plate located in the photoreaction vessel cavity; in the flow photoreaction vessel, the structure of the photoreaction vessel body is a coiled tube structure. The photoreaction vessel body includes a coiled tube microchannel, and the two ports of the coiled tube microchannel are respectively a second sample inlet and a second sample outlet. The flow photoreaction vessel further includes a raw material storage bottle, a product collection bottle, and an infusion pump. The raw material storage bottle is connected to the second sample inlet through the infusion pump, and the product collection bottle is connected to the second sample outlet. A gas guide tube is provided in the raw material storage bottle; the photoreaction vessel further includes a condensate inlet and a condensate outlet that communicate with the condensation component.
[0016] In a second aspect, the present disclosure provides a photoreaction method applied to the above-mentioned photoreaction device. The photoreaction method includes: preparing a photoreaction solution and transferring the photoreaction solution into the photoreaction vessel; according to the absorption spectrum of the photoreaction solution, controlling the light source system through the control system to adjust the first parameter of the target light source, and controlling the photoreaction vessel through the control system to adjust the second parameter for photoreaction, and starting the light source system to perform photoreaction.
[0017] In some embodiments, it further includes: according to the absorption spectrum of the photoreaction solution, controlling the light source system through the control system to adjust the light intensity of the target light source to a fixed light intensity, controlling the light source system through the control system to sequentially adjust the wavelength of the target light source to a plurality of different test wavelengths, sequentially starting the light source system to carry out photoreaction, and sequentially quantitatively detecting the yield of the target product and calculating the selectivity of the photoreaction; establishing the dependence relationship between the yield and selectivity of the target product and the wavelength of the target light source, and determining the preferred wavelength of the target light source for carrying out photoreaction; controlling the light source system through the control system to adjust the wavelength of the target light source to the preferred wavelength, controlling the light source system through the control system to sequentially adjust the light intensity of the target light source to a plurality of different test light intensities, sequentially starting the light source system to carry out photoreaction, and sequentially quantitatively detecting the yield of the target product and calculating the selectivity of the photoreaction; establishing the dependence relationship between the yield and selectivity of the target product and the light intensity of the target light source, and determining the preferred light intensity of the target light source for carrying out photoreaction; controlling the light source system through the control system to adjust the wavelength of the target light source to the preferred wavelength, controlling the light source system through the control system to adjust the light intensity of the target light source to the preferred light intensity, controlling the photoreaction vessel through the control system to adjust the second parameter for carrying out photoreaction, sequentially starting the light source system to carry out photoreaction, and sequentially quantitatively detecting the yield of the target product and calculating the selectivity of the photoreaction; establishing the dependence relationship between the yield and selectivity of the target product and the second parameter, and determining the preferred second parameter for carrying out photoreaction.
[0018] In some embodiments, the photoreaction vessel includes a photoreaction vessel body and a condensation component. The condensation component is a cavity structure including a groove that fits the shape of the photoreaction vessel body. The cavity of the condensation component is used to hold the condensate. The photoreaction vessel body is embedded in the groove, and the photoreaction vessel body is used to hold the photoreaction liquid. The photoreaction vessel includes a non-flow photoreaction vessel and a flow photoreaction vessel. In the non-flow photoreaction vessel, the photoreaction vessel body includes a photoreaction vessel cavity, and the structure of the photoreaction vessel cavity is a flat and hollow three-dimensional structure. The non-flow photoreaction vessel further includes a first sample inlet, a first sample outlet, a first gas inlet that communicates with the photoreaction vessel cavity, and a sand plate located inside the photoreaction vessel cavity. In the flow photoreaction vessel, the structure of the photoreaction vessel body is a coiled tube structure. The photoreaction vessel body includes a coiled tube microchannel, and the two ports of the coiled tube microchannel are respectively a second sample inlet and a second sample outlet. The flow photoreaction vessel further includes a raw material storage bottle, a product collection bottle, and an infusion pump. The raw material storage bottle is connected to the second sample inlet through the infusion pump, and the product collection bottle is connected to the second sample outlet. A gas guide tube is provided in the raw material storage bottle. The photoreaction vessel further includes a condensate inlet and a condensate outlet that communicate with the condensation component. The photoreaction method further includes: selecting a non-flow photoreaction vessel or a flow photoreaction vessel as the photoreaction vessel for carrying out the photoreaction; when selecting a non-flow photoreaction vessel as the photoreaction vessel for carrying out the photoreaction, controlling the photoreaction vessel through a control system to adjust the temperature and gas flow rate for carrying out the photoreaction; when selecting a flow photoreaction vessel as the photoreaction vessel for carrying out the photoreaction, controlling the photoreaction vessel through a control system to adjust the temperature, gas flow rate, and photoreaction liquid flow rate for carrying out the photoreaction.
[0019] The technical solution provided by the present disclosure has the following advantages compared with the prior art:
[0020] The photoreaction equipment provided by the present disclosure can adjust the first parameter of the target light source and the second parameter for carrying out the photoreaction, optimize the first parameter of the target light source and the second parameter for carrying out the photoreaction, that is, screen the better photoreaction parameters, so as to improve the photon utilization rate, achieve the purpose of synthesizing the target product with high yield and high selectivity, and can also improve the photochemical quantum yield, shorten the reaction time, maximize the yield of the photoreaction product, and at the same time have high efficiency. At the same time, the photoreaction equipment can flexibly adjust various parameters of the photoreaction according to different photoreaction requirements, is applicable to various types of photoreactions, and has flexibility and universality.
[0021] Correspondingly, the photoreaction method provided by the present disclosure also has the above technical effects. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] The accompanying drawings herein are incorporated into and constitute a part of this specification, showing embodiments consistent with the present disclosure and, together with the specification, are used to explain the principles of the present disclosure.
[0023] To more clearly illustrate the technical solutions in the embodiments of the present disclosure or the prior art, the following will briefly introduce the accompanying drawings required for use in the description of the embodiments or the prior art. Obviously, for those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.
[0024] Figure 1 It is a schematic structural diagram of a photoreaction device provided by the present disclosure;
[0025] Figure 2 It is a schematic structural diagram of a light source assembly provided by the present disclosure;
[0026] Figure 3 It is a schematic structural diagram of a photoreaction vessel provided by the present disclosure;
[0027] Figure 4 It is a schematic flowchart of a photoreaction method provided by the present disclosure.
[0028] Reference numerals: 10, light source system; 11, light source assembly; 111, fundamental frequency light source; 112, optical reflector; 113, optical lens; 114, optical frequency conversion crystal; 12, beam shaping module; 20, photoreaction vessel; 20a, non-flowing photoreaction vessel; 20b, flowing photoreaction vessel; 21, photoreaction vessel body; 21a, photoreaction vessel cavity; 21b, coiled microchannel; 211, first sample inlet; 212, first sample outlet; 213, first gas 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 embodiments
[0029] In order to be able to more clearly understand the above objects, features, and advantages of the present disclosure, the following will further describe the solutions of the present disclosure. It should be noted that, without conflict, the embodiments of the present disclosure and the features in the embodiments can be combined with each other.
[0030] Many specific details are set forth in the following description to facilitate a thorough understanding of the present disclosure, but the present disclosure can also be implemented in other ways different from those described herein; obviously, the embodiments in the specification are only some embodiments of the present disclosure, rather than all embodiments.
[0031] Figure 1 This is a schematic structural diagram of a photoreaction device provided by the present disclosure. Refer to Figure 1 , embodiments of the present disclosure provide a photoreaction device, which includes:
[0032] A light source system 10, which is used to provide a target light source required for photoreaction, and the spectral range of the target light source includes the ultraviolet light region, the visible light region, and the infrared light region;
[0033] A photoreaction vessel 20, which is used to contain a photoreaction solution to be subjected to photoreaction;
[0034] A control system 30, which is electrically connected to the light source system 10 and the photoreaction vessel 20. The control system 30 is used to control the light source system 10 to adjust a first parameter of the target light source, and the first parameter includes one or more of wavelength, light intensity, spot size, spot shape, and irradiation direction. Moreover, the control system 30 is also used to control the photoreaction vessel 20 to adjust a second parameter for performing photoreaction, and the second parameter includes at least one or more of temperature, gas flow rate, and photoreaction solution flow rate.
[0035] Specifically, embodiments of the present disclosure provide a photoreaction device, which includes a light source system 10, a photoreaction vessel 20, and a control system 30. Among them, the light source system 10 is used to provide a target light source required for photoreaction, that is, the light source system 10 is used to provide the light energy required for photoreaction to the photoreaction vessel 20. The light source system 10 is arranged outside the photoreaction vessel 20, and the light source system 10 belongs to an external illumination type light source. The light source provided by the light source system 10 vertically enters the photoreaction solution from the side, top, or bottom of the photoreaction vessel 20. The photoreaction vessel 20 is used to contain a photoreaction solution to be subjected to photoreaction, that is, the photoreaction vessel 20 can be used to contain the photoreaction solution and provide a place for the photoreaction solution to perform photoreaction.
[0036] The spectral range of the target light source provided by the light source system 10 includes the ultraviolet light region, the visible light region, and the infrared light region, and can cover a wide range of photoreaction categories. In some optional embodiments, the spectral range of the target light source provided by the light source system 10 is 230 - 1080 nanometers, including the ultraviolet light region (230 - 400 nanometers), the visible light region (400 - 760 nanometers), and the infrared light region (760 - 1080 nanometers), and can cover a wide range of photoreaction categories.
[0037] The control system 30 is electrically connected to the light source system 10 and the photoreaction vessel 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, spot size, 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 the first parameters of the target light source. The control system 30 is also used to control the photoreaction vessel 20 to adjust the second parameters for carrying out the photoreaction. The second parameters at least include 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 carrying out the photoreaction and control the photoreaction vessel 20 to adjust the second parameters for carrying out the photoreaction. That is, for a specific photoreaction, the photoreaction device can adjust the first parameters of the target light source and the second parameters for carrying out the photoreaction, optimize the first parameters of the target light source and the second parameters for carrying out the photoreaction, that is, screen out better photoreaction parameters, so as to improve the photon utilization rate, achieve the purpose of high-yield and high-selectivity synthesis of the target product, and can also improve the photoluminescence quantum yield, shorten the reaction time, maximize the yield of the photoreaction product, and at the same time have high efficiency. At the same time, the photoreaction device can flexibly adjust the parameters of the photoreaction according to different photoreaction requirements, is applicable to various types of photoreactions, and has flexibility and universality.
[0038] In some alternative embodiments, the control system 30 includes a parameter adjustment interface, and the parameter adjustment interface can be used to adjust the first parameters of the target light source and the second parameters for carrying out the photoreaction. Exemplarily, the parameter adjustment interface can be a display screen.
[0039] In some alternative embodiments, the light source system 10 can be used to feedback the first parameters of the target light source to the control system 30, the photoreaction vessel 20 can be used to feedback the second parameters for carrying out the photoreaction to the control system 30, and the control system 30 can be used to monitor the operating state of the photoreaction device in real time.
[0040] In some alternative embodiments, the control system 30 further includes an alarm module, and the alarm module can be used to give a fault alarm when there is a problem with the operation of the photoreaction device.
[0041] Figure 2 is a schematic structural diagram of a light source assembly provided by the present disclosure. Refer to Figure 1 and Figure 2 , in some alternative embodiments, the light source system 10 includes a light source assembly 11 and a beam shaping module 12;
[0042] The light source assembly 11 is used to adjust the wavelength and light intensity of the target light source. The light source assembly 11 includes a fundamental frequency light source 111, an optical mirror 112, an optical lens 113, and an optical frequency conversion crystal 114. The fundamental frequency light source 111 is used to emit a light source in the first spectral range. The light beam emitted by the fundamental frequency light source 111 is partially reflected by the optical lens 113 and then directed towards the optical mirror 112, and after being reflected by the optical mirror 112, it is converted into a light source in the second spectral range by the optical frequency conversion crystal 114. The first spectral range and the second spectral range partially do not overlap;
[0043] The beam shaping module 12 includes a spot homogenizer (not shown in the figure), a spot shape and size regulator (not shown in the figure), and a beam direction regulator (not shown in the figure). The spot homogenizer is used to homogenize the light intensity of the target light source. The spot shape and size regulator is used to adjust the spot size and spot shape of the target light source. The beam direction regulator is used to adjust the beam propagation direction of the target light source.
[0044] Specifically, the light source system 10 includes a light source assembly 11, and the light source assembly 11 is used to adjust the wavelength and light intensity of the target light source. The light source assembly 11 includes a fundamental frequency light source 111, an optical mirror 112, an optical lens 113, and an optical frequency conversion crystal 114. The fundamental frequency light source 111 is used to emit a light source in the first spectral range. The light beam emitted by the fundamental frequency light source 111 is partially directly emitted through the optical lens 113, so that the light source assembly 11 can emit the fundamental frequency light source in the first spectral range. Optionally, the fundamental frequency light source 111 can be a laser light source, and the laser light source has strong monochromaticity, and the light wavelength and light intensity can be precisely tuned. Optionally, the fundamental frequency light source 111 can be a titanium 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 beam emitted by the fundamental frequency light source 111 is partially reflected by the optical lens 113 and then directed towards the optical mirror 112, and then after being reflected by the optical mirror 112, it is converted into a frequency-converted light source in the second spectral range by the optical frequency conversion crystal 114. The first spectral range and the second spectral range partially do not overlap. The second spectral range can be 230 - 680 nanometers. Thus, the spectral range of the target light source provided by the light source assembly 11 can be 230 - 1080 nanometers, including the ultraviolet light region (230 - 400 nanometers), the visible light region (400 - 760 nanometers), and the infrared light region (760 - 1080 nanometers), and can cover a wide range of photoreaction categories.
[0045] Optionally, the target light source can be continuously adjustable within the spectral range of 230 - 1080 nanometers, the full width at half maximum of a single wavelength ≤ 0.1 nanometer, and the light intensity can be continuously adjustable within the range of 0 - 100 milliwatts.
[0046] In some alternative embodiments, the optical frequency conversion crystal 114 may 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.
[0047] The light source system 10 includes a beam shaping module 12. The beam shaping module 12 includes a spot homogenizer, a spot shape and size adjuster, and a beam direction adjuster. The spot homogenizer is used to homogenize the light intensity of the target light source. The spot shape and size adjuster is used to adjust the spot size and spot shape of the target light source. The beam direction adjuster is used to adjust the beam propagation direction of the target light source. Thus, the light intensity of the target light source is optimized, the spot size and spot shape of the target light source are adjusted, and the beam propagation direction of the target light source is changed through the beam shaping module 12.
[0048] That is, the adjustment of the wavelength of the target light source is achieved through the setting of the light source assembly 11, and it can be adjusted to the preferred wavelength, making the target product of the reaction have higher yield and higher selectivity. And through the settings of the light source assembly 11 and the beam shaping module 12, the light intensity, spot size, spot shape, and propagation direction of the target light source are adjusted, and each parameter is adjusted to the optimal value, effectively improving the photon yield, shortening the reaction time, maximizing the yield of the photoreaction product, and being efficient at the same time.
[0049] In some alternative embodiments, the spot homogenizer includes one or more of a microlens array, a molecular sieve, a soft-edge aperture, an aberration-corrected shaping lens group, and a square optical fiber, and can homogenize the Gaussian-distributed light intensity into a flat-top distribution, thereby achieving the homogenization of the light intensity of the target light source. Of course, in other embodiments of the present disclosure, the spot homogenizer may also include other spot homogenizers, which are not elaborated herein one by one.
[0050] In some alternative embodiments, the spot shape and size adjuster includes one or more of an expansion and collimation lens group, a cylindrical lens, a square aperture, and an aberration-corrected shaping lens group, and can adjust the shape and size of the spot formed by the target light source, convert the dot-shaped spot into circles, squares, ellipses, spindles, etc. of different sizes, so that the shape and size of the spot formed by the target light source match the photoreaction vessel. Of course, in other embodiments of the present disclosure, the spot shape and size adjuster may also include other spot shape and size adjusters, which are not elaborated herein one by one.
[0051] In some alternative embodiments, the beam direction adjuster includes one or more of a beam turning unit, a fiber collimation lens group, and an optical fiber, and can change the propagation direction of the light source emitted by the light source assembly, forming top-illumination, side-illumination, bottom-illumination, etc. modes, thereby achieving the adjustment of the propagation direction of the target light source, so that the beam formed by the target light source can vertically enter the interior of the photoreaction vessel.
[0052] Figure 3 is a schematic structural diagram of a photoreaction vessel provided by the present disclosure. Refer to Figure 1 and Figure 3 , in some alternative embodiments, the photoreaction vessel 20 includes a photoreaction vessel main body 21 and a condensation component 22. The condensation component 22 is a cavity structure including a groove that fits the shape of the photoreaction vessel main body 21. The cavity of the condensation component 22 is used to accommodate the condensate. The photoreaction vessel main body 21 is embedded in the groove, and the photoreaction vessel main body 21 is used to accommodate the photoreaction liquid.
[0053] Specifically, the photoreaction vessel 20 includes a photoreaction vessel main body 21 and a condensation component 22. The photoreaction vessel main body 21 is used to accommodate the photoreaction liquid. Optionally, the material of the photoreaction vessel main body 21 can be quartz glass with high light transmittance. The condensation component 22 is a cavity structure including a groove that fits the shape of the photoreaction vessel main body 21, so that the photoreaction vessel main 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 accommodate the condensate, for controlling the temperature of the photoreaction.
[0054] Continue to refer to Figure 1 and Figure 3 , in some alternative embodiments, the photoreaction vessel 20 includes a non-flow photoreaction vessel 20a and a flow photoreaction vessel 20b;
[0055] In the non-flow photoreaction vessel 20a, the photoreaction vessel main body 21 includes a photoreaction vessel cavity 21a. The structure of the photoreaction vessel cavity 21a is a flat and hollow three-dimensional structure. The non-flow photoreaction vessel 20a further includes a first sample inlet 211, a first sample outlet 212, a first gas inlet 213 that communicate with the photoreaction vessel cavity 21a, and a sand plate 214 located inside the photoreaction vessel cavity 21a;
[0056] In the flow photoreaction vessel 20b, the structure of the photoreaction vessel main body 21 is a coiled tube structure. The photoreaction vessel main body 21 includes a coiled tube microchannel 21b. The two ports of the coiled tube microchannel 21b are respectively a second sample inlet 215 and a second sample outlet 216. The flow photoreaction vessel 20b further includes a raw material storage bottle 217, a product collection bottle 218, and an infusion pump 219. The raw material storage bottle 217 is connected to the second sample inlet 215 through the infusion pump 219. The product collection bottle 218 is connected to the second sample outlet 216. A gas guide tube 2110 is provided in the raw material storage bottle 217;
[0057] The photoreaction vessel 20 further includes a condensate inlet 221 and a condensate outlet 222 that communicate with the condensation component 22.
[0058] Specifically, the photoreaction vessel 20 includes at least two types of photoreaction vessels, including a non-flow photoreaction vessel 20a and a flow photoreaction vessel 20b. Of course, in other embodiments of the present disclosure, the photoreaction vessel 20 may also include other types of photoreaction vessels, which will not be elaborated herein one by one.
[0059] In the non-flow photoreaction vessel 20a, the photoreaction vessel main body 21 includes a photoreaction vessel cavity 21a, and the structure of the photoreaction vessel cavity 21a is a flat and hollow three-dimensional structure. The non-flow photoreaction vessel 20a further includes a first sample inlet 211, a first sample outlet 212, a first gas inlet 213 that communicate with the photoreaction vessel cavity 21a, and a sand plate 214 located inside the photoreaction vessel cavity 21a. The photoreaction liquid enters the photoreaction vessel cavity 21a through the first sample inlet 211, and the gas enters the photoreaction vessel cavity 21a through the first gas inlet 213. A sand plate 214 is provided inside the photoreaction vessel cavity 21a, and the first sample inlet 211 and the first sample outlet 212 are located on one side of the sand plate 214, while the first gas inlet 213 is located on the other side of the sand plate 214. During the photoreaction, stable bubbles can be formed by using the sand plate 214 to disturb the photoreaction liquid, achieving the purpose of mass transfer and heat transfer and balancing the photoreaction. The beam of the target light source enters the photoreaction vessel cavity 21a perpendicularly to the side with the largest area of the non-flow photoreaction vessel 20a, and the photoreaction liquid can be exported through the first sample outlet 212 after the photoreaction.
[0060] In the flow photoreaction vessel 20b, the structure of the photoreaction vessel main body 21 is a coiled tube structure, and the photoreaction vessel main body 21 includes a coiled tube microchannel 21b. Optionally, the coiled tube microchannel 21b can be a microchannel with an inner diameter not exceeding 2 mm. The two ports of the coiled tube microchannel 21b are respectively a second sample inlet 215 and a second sample outlet 216. The flow photoreaction vessel 20b further includes a raw material storage bottle 217, a product collection bottle 218, and an infusion pump 219. The raw material storage bottle 217 is connected to the second sample inlet 215 through the infusion pump 219, and the product collection bottle 218 is connected to the second sample outlet 216. An air duct 2110 is provided in the raw material storage bottle 217. The volume of the photoreaction liquid in the flow photoreaction vessel 20b is not fixed. The photoreaction liquid is stored in the raw material storage bottle 217, and the gas enters the raw material storage bottle 217 through the air duct 2110. The infusion pump 219 pushes the photoreaction liquid from the raw material storage bottle 217 into the coiled tube microchannel 21b continuously from the second sample inlet 215 at a certain speed. During the flow process, the photoreaction liquid is automatically disturbed and mixed. The beam of the target light source enters the coiled tube microchannel 21b perpendicularly to the plane of the non-flow photoreaction vessel 20a, and the photoreaction liquid flows out through the second sample outlet 216 after the photoreaction and enters the product collection bottle 218.
[0061] The photoreaction vessel 20 further includes a liquid inlet 221 and a liquid outlet 222 that communicate with the condensation component 22. The condensate enters the condensation component 22 through the condensate liquid inlet 221 and is discharged from the condensation component 22 through the condensate liquid outlet 222. The temperature of the photoreaction is controlled by controlling the flow rate of the condensate.
[0062] The photoreaction vessel 20 includes a non-flowing photoreaction vessel 20a and a flowing photoreaction vessel 20b. The non-flowing photoreaction vessel 20a is suitable for performing photoreactions on a photoreaction liquid of a determined volume, and the flowing photoreaction vessel 20b is suitable for performing photoreactions on a photoreaction liquid of an open volume, which can be applied to different photoreaction scenarios.
[0063] An embodiment of the present disclosure provides a photoreaction method, which is applied to the above-mentioned photoreaction device. Figure 4 It is a schematic flow chart of a photoreaction method provided by the present disclosure. Refer to Figure 4 , the photoreaction method includes:
[0064] Step S100, configure the photoreaction liquid and transfer the photoreaction liquid to the photoreaction vessel.
[0065] Step S200, according to the absorption spectrum of the photoreaction liquid, control the light source system through the control system to adjust the first parameter of the target light source, and control the photoreaction vessel through the control system to adjust the second parameter for performing the photoreaction, and start the light source system to perform the photoreaction.
[0066] Specifically, in combination with Figure 1 and Figure 4 , the photoreaction method provided in this embodiment is applied to a photoreaction device. Among them, the photoreaction device includes a light source system 10, a photoreaction vessel 20, and a control system 30. The light source system 10 is used to provide the target light source required for the photoreaction, that is, the light source system 10 is used to provide the light energy required for the photoreaction to the photoreaction vessel 20. The light source system 10 is arranged outside the photoreaction vessel 20. The light source system 10 belongs to an external illumination type light source, and the light source provided by the light source system 10 vertically enters the photoreaction liquid from the side, top, or bottom of the photoreaction vessel 20. The photoreaction vessel 20 is used to accommodate the photoreaction liquid to be subjected to the photoreaction, that is, the photoreaction vessel 20 can be used to accommodate the photoreaction liquid and provide a place for the photoreaction liquid to perform the photoreaction.
[0067] The spectral range of the target light source provided by the light source system 10 includes the ultraviolet region, the visible region, and the infrared region, and can cover a wide range of photochemical reaction categories. In some alternative embodiments, the spectral range of the target light source provided by the light source system 10 is 230 - 1080 nanometers, including the ultraviolet region (230 - 400 nanometers), the visible region (400 - 760 nanometers), and the infrared region (760 - 1080 nanometers), and can cover a wide range of photochemical reaction categories.
[0068] The control system 30 is electrically connected to the light source system 10 and the photoreaction vessel 20. The control system 30 is used to control the light source system 10 to adjust a first parameter of the target light source, and the first parameter includes one or more of wavelength, light intensity, spot size, spot shape, and irradiation direction. The control system 30 is further used to control the photoreaction vessel 20 to adjust a second parameter for carrying out the photochemical reaction, and the second parameter at least includes one or more of temperature, gas flow rate, and photoreaction liquid flow rate.
[0069] In the photochemical reaction method provided in this embodiment, the photoreaction liquid can be first configured and transferred to the photoreaction vessel 20. Then, according to the absorption spectrum of the photoreaction liquid, the control system 30 is used to control the light source system 10 to adjust the first parameter of the target light source, and the control system 30 is used to control the photoreaction vessel 20 to adjust the second parameter for carrying out the photochemical reaction. Then, the light source system 10 is started to carry out the photochemical reaction. That is, in the photochemical reaction method provided in this embodiment, for a specific photochemical reaction, the photochemical reaction device can adjust the first parameter of the target light source and the second parameter for carrying out the photochemical reaction, optimize the first parameter of the target light source and the second parameter for carrying out the photochemical reaction, that is, screen out relatively better photochemical reaction parameters, so as to improve the photon utilization rate, achieve the purpose of high-yield and high-selectivity synthesis of the target product, and can also improve the photonic yield, shorten the reaction time, maximize the yield of the photoreaction product, and at the same time have high efficiency. At the same time, the photochemical reaction device can flexibly adjust various parameters of the photochemical reaction according to different photochemical reaction requirements, is applicable to various types of photochemical reactions, and has flexibility and universality.
[0070] In some alternative embodiments, the photochemical reaction further includes:
[0071] According to the absorption spectrum of the photoreaction liquid, the control system is used to control the light source system to adjust the light intensity of the target light source to a fixed light intensity, and the control system is used to control the light source system to sequentially adjust the wavelength of the target light source to a plurality of different test wavelengths, respectively start the light source system to carry out the photochemical reaction in sequence, and sequentially quantitatively detect the yield of the target product and calculate the selectivity of the photochemical reaction.
[0072] That is, according to the absorption spectrum of the photoreaction solution, the control system controls the light source system to adjust the light intensity of the target light source to a fixed light intensity W0. According to the ultraviolet-visible absorption spectrum of the photoreaction solution, the wavelengths of the target light source are set as λ1, λ2, λ3, λ4, etc. in sequence, and the above process of the photoreaction method is repeated to complete the photoreaction under each wavelength of light, and the yield of the target product is quantitatively detected in sequence, and the selectivity of the photoreaction is calculated.
[0073] Establish the dependence relationship between the yield and selectivity of the target product and the wavelength of the target light source, and determine the preferred wavelength λ of the target light source for carrying out the photoreaction. max 。
[0074] The control system controls the light source system to adjust the wavelength of the target light source to the preferred wavelength, and the control system controls the light source system to sequentially adjust the light intensity of the target light source to multiple different test light intensities, and the light source system is sequentially started to carry out the photoreaction, and the yield of the target product is quantitatively detected in sequence, and the selectivity of the photoreaction is calculated.
[0075] That is, fix the preferred wavelength λ of the target light source. max Set the light intensities of the target light source as W1, W2, W3, W4, etc. in sequence, and repeat the above process of the photoreaction method to complete the photoreaction under each wavelength of light, and the yield of the target product is quantitatively detected in sequence, and the selectivity of the photoreaction is calculated.
[0076] Establish the dependence relationship between the yield and selectivity of the target product and the light intensity of the target light source, and determine the preferred light intensity W of the target light source for carrying out the photoreaction. max 。
[0077] The control system controls the light source system to adjust the wavelength of the target light source to the preferred wavelength, the control system controls the light source system to adjust the light intensity of the target light source to the preferred light intensity, and the control system controls the photoreaction vessel to adjust the second parameter for carrying out the photoreaction. The light source system is sequentially started to carry out the photoreaction, and the yield of the target product is quantitatively detected in sequence, and the selectivity of the photoreaction is calculated.
[0078] That is, when fixing the preferred wavelength λ of the target light source. max and fixing the preferred light intensity W of the target light source. max Optimize parameters such as the temperature, concentration of the reaction solution, gas flow rate, and flow rate of the photoreaction solution for carrying out the photoreaction, and quantitatively detect the yield of the target product in sequence, and calculate the selectivity of the photoreaction.
[0079] Establish the dependence relationship between the yield and selectivity of the target product and the second parameter, and determine the preferred second parameter for carrying out the photoreaction.
[0080] The photochemical reaction method provided by this embodiment can accurately screen and determine the preferred wavelength of the target light source for the photochemical reaction, making the target product of the reaction have higher yield and selectivity. Moreover, by optimizing the light intensity, spot shape and size, the photonic yield is effectively improved, the reaction time is shortened, the yield of the photoreaction product is maximized, and high efficiency is achieved at the same time.
[0081] Optionally, during the photochemical reaction process, thin-layer chromatography, high-pressure liquid chromatography, gas chromatography, etc. can be used to monitor the progress of the photochemical reaction in real time. High-pressure liquid chromatography, nuclear magnetic resonance hydrogen spectrum, gas chromatography, etc. can be used to quantitatively detect the yield of the target product and calculate the selectivity of the photochemical reaction.
[0082] In some alternative embodiments, referring to Figure 1 and Figure 3 , the photoreaction vessel 20 includes a photoreaction vessel main body 21 and a condensation component 22. The condensation component 22 is a cavity structure including a groove that fits the shape of the photoreaction vessel main body 21. The cavity of the condensation component 22 is used to hold the condensate. The photoreaction vessel main body 21 is embedded in the groove, and the photoreaction vessel main body 21 is used to hold the photoreaction solution. The photoreaction vessel 20 includes a non-flowing photoreaction vessel 20a and a flowing photoreaction vessel 20b; in the non-flowing photoreaction vessel 20a, the photoreaction vessel main body 21 includes a photoreaction vessel cavity 21a, and the structure of the photoreaction vessel cavity 21a is a flat and hollow three-dimensional structure. The non-flowing photoreaction vessel 20a further includes a first sample inlet 211, a first sample outlet 212, a first gas inlet 213 that communicate with the photoreaction vessel cavity 21a, and a sand plate 214 located inside the photoreaction vessel cavity 21a; in the flowing photoreaction vessel 20b, the structure of the photoreaction vessel main body 21 is a coiled tube structure. The photoreaction vessel main body 21 includes a coiled tube microchannel 21b. The two ports of the coiled tube microchannel 21b are respectively a second sample inlet 215 and a second sample outlet 216. The flowing photoreaction vessel 20b further includes a raw material storage bottle 217, a product collection bottle 218, and an infusion pump 219. The raw material storage bottle 217 is connected to the second sample inlet 215 through the infusion pump 219, and the product collection bottle 218 is connected to the second sample outlet 216. A gas guide tube 2110 is provided in the raw material storage bottle 217; the photoreaction vessel 20 further includes a condensate inlet 221 and a condensate outlet 222 that communicate with the condensation component 22.
[0083] Specifically, the photoreaction vessel 20 includes at least two types of photoreaction vessels, including a non-flowing photoreaction vessel 20a and a flowing photoreaction vessel 20b.
[0084] The photoreaction container body 21 in the non-flow photoreaction container 20a includes a photoreaction container cavity 21a, and the structure of the photoreaction container cavity 21a is a flat hollow three-dimensional structure. The non-flow photoreaction container 20a also includes a first sample inlet 211, a first sample outlet 212 and a first air inlet 213 that are connected to the photoreaction container cavity 21a, and a sand plate 214 located in 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. The sand plate 214 is arranged in the photoreaction container cavity 21a, and the first sample inlet 211 and the first sample outlet 212 are located on one side of the sand plate 214, and the first air inlet 213 is located on the other side of the sand plate 214. When performing a photochemical reaction, the sand plate 214 can be used to form stable bubbles to disturb the photoreaction liquid, thereby achieving the purpose of mass transfer and heat transfer and balancing the photochemical reaction. The light beam of the target light source enters the photoreaction container cavity 21 a perpendicularly to the side surface of the non-flow photoreaction container 20 a with the largest area, and the photoreaction liquid can be discharged through the first sample outlet 212 after undergoing photochemical reaction.
[0085] The structure of the photoreaction container body 21 in the flow-type photoreaction container 20b is a coil-shaped structure, and the photoreaction container body 21 includes a coil microchannel 21b. Optionally, the coil microchannel 21b can be a microchannel with an inner diameter of no more than 2 mm. The two ports of the coil microchannel 21b are respectively a second sample inlet 215 and a second sample outlet 216. The flow-type photoreaction container 20b also includes a raw material storage bottle 217, a product collection bottle 218 and an infusion pump 219, the raw material storage bottle 217 is connected to the second sample inlet 215 through the infusion pump 219, the product collection bottle 218 is connected to the second sample outlet 216, and an air 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. The 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 to enter the coil microchannel 21b from the second sampling port 215 at a certain speed. During the flow process, the photoreaction liquid is automatically disturbed and mixed. The light beam of 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 sampling port 216 and enters the product collection bottle 218.
[0086] The photoreaction container 20 also includes a liquid inlet 221 and a liquid outlet 222 which are connected to the condensation component 22. The condensate enters the condensation component 22 through the liquid inlet 221 and is discharged from the condensation component 22 through the liquid outlet 222. The temperature of the photochemical reaction is controlled by controlling the flow rate of the condensate.
[0087] Photochemical reaction methods also include:
[0088] Select a non-flow type photoreaction vessel or a flow type photoreaction vessel as the photoreaction vessel for carrying out the photoreaction;
[0089] When selecting a non-flow type photoreaction vessel as the photoreaction vessel for carrying out the photoreaction, control the photoreaction vessel through the control system to adjust the temperature and gas flow rate for carrying out the photoreaction;
[0090] When selecting a flow type photoreaction vessel as the photoreaction vessel for carrying out the photoreaction, control the photoreaction vessel through the control system to adjust the temperature, gas flow rate and photoreaction liquid flow rate for carrying out the photoreaction.
[0091] Specifically, since the photoreaction vessel includes a non-flow type photoreaction vessel and a flow type photoreaction vessel, before carrying out the photoreaction, first select a non-flow type photoreaction vessel or a flow type photoreaction vessel as the photoreaction vessel for carrying out the photoreaction. When selecting a non-flow type photoreaction vessel as the photoreaction vessel for carrying out the photoreaction, first introduce gas into the interior of the photoreaction vessel main body, then transfer the photoreaction liquid into the photoreaction vessel main body, start the circulation of the condensate liquid in the condensation component and monitor the temperature of the photoreaction through the control system, and adjust the gas flow rate of the photoreaction through the control system.
[0092] When selecting a flow type photoreaction vessel as the photoreaction vessel for carrying out the photoreaction, first transfer the photoreaction liquid into the raw material storage bottle, then introduce the gas participating in the photoreaction into the raw material storage bottle, start the circulation of the condensate liquid in the condensation component and monitor the temperature of the photoreaction through the control system, start the infusion pump, continuously input the photoreaction liquid into the photoreaction vessel main body, enter the product collection bottle after the photoreaction by light irradiation, and adjust the gas flow rate and photoreaction liquid flow rate of the photoreaction through the control system.
[0093] Exemplarily, this embodiment provides a specific example of precisely optimizing the parameters of the photoreaction for generating previtamin D2 from ergosterol by using the above photoreaction equipment:
[0094] At room temperature of 25 °C, dissolve 2.4 grams of ergosterol in a mixed solvent of 500 milliliters of methanol and n-hexane (methanol: n-hexane = 3:1) to prepare a photoreaction liquid.
[0095] Start the control system, configure a non-flowing photoreaction vessel, and set the side-illumination mode. Set the nitrogen gas flow rate to 1 liter per minute, the temperature of the condensation component to 20 °C, the wavelength of the target light source to 273 nm, the light intensity to 220 mW, and the spot size to a 5×6 square centimeter rectangle. Turn on the nitrogen gas and the condensation component, and transfer 20 ml of the photoreaction solution to the non-flowing photoreaction vessel. Start the light source system. After 30 minutes of light irradiation reaction, end the photochemical reaction. Use high-performance liquid chromatography to detect the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 90.2%, previtamin D2 9.1%, tachysterol 0.6%, vitamin D2 0.1%.
[0096] In the above operation, switch the wavelength of the target light source to 282 nm, keep other conditions unchanged. After 30 minutes of light irradiation reaction, end the photochemical reaction. Use high-performance liquid chromatography to detect the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 66.7%, previtamin D2 27.2%, tachysterol 5.9%, lumisterol 0.1%, vitamin D2 0.1%.
[0097] In the above operation, switch the wavelength of the target light source to 289 nm, keep other conditions unchanged. After 30 minutes of light irradiation reaction, end the photochemical reaction. Use high-performance liquid chromatography to detect the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 19.2%, previtamin D2 55.6%, tachysterol 23.9%, lumisterol 1.1%, vitamin D2 0.2%.
[0098] In the above operation, switch the wavelength of the target light source to 300 nm, keep other conditions unchanged. After 30 minutes of light irradiation reaction, end the photochemical reaction. Use high-performance liquid chromatography to detect the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 4.9%, previtamin D2 71.6%, tachysterol 20.6%, lumisterol 2.8%, vitamin D2 0.1%.
[0099] In the above operation, switch the wavelength of the target light source to 304 nm, keep other conditions unchanged. After 30 minutes of light irradiation reaction, end the photochemical reaction. Use high-performance liquid chromatography to detect the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 14.6%, previtamin D2 61.4%, tachysterol 17.5%, lumisterol 6.2%, vitamin D2 0.2%.
[0100] In the above operation, switch the wavelength of the target light source to 300 nm, adjust the light intensity to 100 mW, keep other conditions unchanged. After 20 minutes of light irradiation reaction, end the photochemical reaction. Use high-performance liquid chromatography to detect the photoreaction solution and determine the product distribution under these reaction conditions: ergosterol 68.3%, previtamin D2 28.5%, tachysterol 3.2%.
[0101] 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 light irradiation reaction, the photochemical reaction was terminated. The photoreaction solution was detected by high-pressure liquid phase to determine the product distribution under this reaction condition: ergosterol 49.6%, previtamin D2 44.7%, tachysterol 5.6%, lumisterol 0.2%.
[0102] 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 light irradiation reaction, the photochemical reaction was terminated. The photoreaction solution was detected by high-pressure liquid phase to determine the product distribution under this reaction condition: ergosterol 37.5%, previtamin D2 53.2%, tachysterol 8.5%, lumisterol 0.7%, vitamin D2 0.1%.
[0103] 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 light irradiation reaction, the photochemical reaction was terminated. The photoreaction solution was detected by high-pressure liquid phase to determine the product distribution under this reaction condition: ergosterol 24.6%, previtamin D2 61.8%, tachysterol 12.1%, lumisterol 1.4%, vitamin D2 0.1%.
[0104] 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 light irradiation reaction, the photochemical reaction was terminated. The photoreaction solution was detected by high-pressure liquid phase to determine the product distribution under this reaction condition: ergosterol 0.9%, previtamin D2 78.5%, tachysterol 18.6%, lumisterol 1.9%, vitamin D2 0.1%.
[0105] Based on the above data, the parameters of the photochemical reaction for the formation of previtamin D2 from ergosterol can be accurately optimized.
[0106] It should be noted that only an exemplary embodiment of accurately optimizing the parameters of the photochemical reaction for the formation of previtamin D2 from ergosterol using the above photochemical reaction equipment is shown in this embodiment. In other embodiments of the present disclosure, the above photochemical reaction equipment can also be used to implement other photochemical reactions, and the present disclosure does not make specific limitations here.
[0107] Using the photoreaction device provided by this embodiment can accurately screen and determine the preferred wavelength of the target light source for photoreaction, making the target product of the reaction have higher yield and selectivity. Moreover, by optimizing the light intensity, spot shape and size, the photoreaction device effectively improves the photon yield, shortens the reaction time, maximizes the yield of photoreaction products, and is efficient at the same time. Meanwhile, the photoreaction device can flexibly adjust various parameters of the photoreaction according to different photoreaction requirements, is applicable to various types of photoreactions, and has flexibility and universality.
[0108] The above description is only a preferred embodiment of the present disclosure and an explanation of the applied technical principles. Those skilled in the art should understand that the scope of disclosure involved in the present disclosure is not limited to the technical solutions formed by the specific combination of the above technical features, and should also cover other technical solutions formed by any combination of the above technical features or their equivalent features without departing from the above disclosure concept. For example, the technical solutions formed by mutually replacing the above features with the technical features (but not limited to) having similar functions disclosed in the present disclosure.
[0109] In addition, although the operations are depicted in a particular order, this should not be construed as requiring that the operations be performed in the particular order shown or in sequential order. In certain circumstances, multitasking and parallel processing may be advantageous. Similarly, although several specific implementation details are included in the above discussion, these should not be construed as limiting the scope of the present disclosure. Certain features described in the context of separate embodiments may also be implemented combinatorially in a single embodiment. Conversely, the various features described in the context of a single embodiment may also be implemented separately or in any suitable sub-combination in multiple embodiments.
[0110] Although the subject matter has been described in language specific to structural features and / or methodological logical acts, it should be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or acts described above. On the contrary, the specific features and acts described above are merely example forms for implementing the claims.
[0111] The above are only specific implementation manners of the present disclosure, enabling those skilled in the art to understand or implement the present disclosure. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present disclosure. Therefore, the present disclosure will not be limited to these embodiments described herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A photochemical reaction device, characterized in that: include: A light source system, wherein the light source system is used to provide a target light source required for a photochemical reaction, and the spectral range of the target light source includes an ultraviolet light region, a visible light region, and an infrared light region; A photoreaction container, the photoreaction container is used to contain a photoreaction liquid to be subjected to a photochemical reaction; A control system, wherein the control system is electrically connected to the light source system and the photoreaction container, and the control system is used to control the light source system to adjust a first parameter of the target light source, wherein the first parameter includes one or more of wavelength, light intensity, spot size, spot shape and irradiation direction, and the control system is also used to control the photoreaction container to adjust a second parameter for photochemical reaction, wherein the second parameter includes at least one or more of temperature, gas flow rate and photoreaction liquid flow rate.
2. The photochemical reaction device according to claim 1, characterized in that: The light source system includes a light source assembly and a beam shaping module; The light source assembly is used to adjust the wavelength and light intensity of the target light source. The light source assembly includes a fundamental frequency light source, an optical reflector, 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 emitted to the optical reflector. After being reflected by the optical reflector, the light beam 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 in part. The beam shaping module includes a spot homogenizer, a spot shape size regulator and a beam direction regulator. The spot homogenizer is used to homogenize the light intensity of the target light source, the spot shape size regulator is used to adjust the spot size and spot shape of the target light source, and the beam direction regulator is used to adjust the beam propagation direction of the target light source.
3. The photochemical reaction device according to claim 2, characterized in that: The light spot homogenizer includes one or more of a microlens array, a molecular sieve, a soft-edge aperture, an aberration shaping lens group and a square optical fiber.
4. The photochemical reaction device according to claim 2, characterized in that: The light spot shape size adjuster includes one or more of a beam expanding collimating lens group, a cylindrical lens, a square aperture and an aberration shaping lens group.
5. The photochemical reaction device according to claim 2, characterized in that: The beam direction regulator includes one or more of a beam turning unit, a fiber collimating lens group and an optical fiber.
6. The photochemical reaction device according to claim 1, characterized in that: The photoreaction container comprises a photoreaction container body and a condensation component. The condensation component is a cavity structure including a groove matching the shape of the photoreaction container body. The cavity of the condensation component is used to accommodate condensate. The photoreaction container body is embedded in the groove. The photoreaction container body is used to accommodate the photoreaction liquid.
7. The photochemical reaction device according to claim 6, characterized in that: The photoreaction container includes a non-flow photoreaction container and a flow photoreaction container; The photoreaction container body in the non-flow photoreaction container comprises a photoreaction container cavity, the structure of the photoreaction container cavity is a flat hollow three-dimensional structure, the non-flow photoreaction container also comprises a first sample inlet, a first sample outlet and a first air inlet which are connected with the photoreaction container cavity, and a sand plate located in the photoreaction container cavity; The photoreaction container comprises a flow-type photoreaction container, wherein the structure of the photoreaction container body in the flow-type photoreaction container is a coil-shaped structure, the photoreaction container body comprises a coil microchannel, and the two ports of the coil microchannel are respectively a second sample inlet and a second sample outlet, the flow-type photoreaction container further comprises a raw material storage bottle, a product collection bottle and an infusion pump, the raw material storage bottle is connected to the second sample inlet through the infusion pump, the product collection bottle is connected to the second sample outlet, and an air guide tube is arranged in the raw material storage bottle; The photoreaction container further comprises a condensate inlet and a condensate outlet which are communicated with the condensation component.
8. A photochemical reaction method, characterized in that: Applied to the photochemical reaction device according to any one of claims 1 to 7, the photochemical reaction method comprises: preparing a photoreaction solution, and transferring the photoreaction solution into a photoreaction container; According to the absorption spectrum of the photoreaction liquid, the control system controls the light source system to adjust the first parameter of the target light source, and the control system controls the photoreaction container to adjust the second parameter of the photochemical reaction, and the light source system is started to perform the photochemical reaction.
9. The photochemical reaction method according to claim 8, characterized in that: Also includes: According to the absorption spectrum of the photoreaction liquid, the control system controls the light source system to adjust the light intensity of the target light source to a fixed light intensity, controls the light source system to sequentially adjust the wavelength of the target light source to a plurality of different test wavelengths, sequentially starts the light source system to perform photochemical reaction, and sequentially quantitatively detects the yield of the target product, and calculates the selectivity of the photochemical reaction; Establishing the dependence of the target product yield and the selectivity on the wavelength of the target light source, and determining the preferred wavelength of the target light source for photochemical reaction; The control system controls the light source system to adjust the wavelength of the target light source to the preferred wavelength, controls the light source system to sequentially adjust the light intensity of the target light source to a plurality of different test light intensities, sequentially starts the light source system to perform photochemical reactions, and sequentially quantitatively detects the yield of the target product, and calculates the selectivity of the photochemical reaction; Establishing the dependence of the target product yield and the selectivity on the light intensity of the target light source, and determining the preferred light intensity of the target light source for the photochemical reaction; Controlling the light source system to adjust the wavelength of the target light source to the preferred wavelength through the control system, controlling the light source system to adjust the light intensity of the target light source to the preferred light intensity through the control system, controlling the light reaction container to adjust a second parameter for a photochemical reaction through the control system, starting the light source systems in sequence to perform a photochemical reaction, and quantitatively detecting the yield of the target product in sequence, and calculating the selectivity of the photochemical reaction; The dependence of the target product yield and the selectivity on the second parameter is established to determine the preferred second parameter for the photochemical reaction.
10. The photochemical reaction method according to claim 8, characterized in that: The photoreaction container comprises a photoreaction container body and a condensation component, wherein the condensation component is a cavity structure comprising a groove matching the shape of the photoreaction container body, the cavity of the condensation component is used to accommodate condensate, the photoreaction container body is embedded in the groove, and the photoreaction container body is used to accommodate the photoreaction liquid; the photoreaction container comprises a non-flow photoreaction container and a flow photoreaction container; the photoreaction container body in the non-flow photoreaction container comprises a photoreaction container cavity, the structure of the photoreaction container cavity is a flat hollow three-dimensional structure, the non-flow photoreaction container also comprises a first injection port, which is communicated with the photoreaction container cavity, A first sample outlet and a first air inlet, and a sand plate located in the cavity of the photoreaction container; the structure of the photoreaction container body in the flow-type photoreaction container is a coil-shaped structure, the photoreaction container body includes a coil microchannel, and the two ports of the coil microchannel are respectively a second sample inlet and a second sample outlet, the flow-type photoreaction container also includes a raw material storage bottle, a product collection bottle and an infusion pump, the raw material storage bottle is connected to the second sample inlet through the infusion pump, the product collection bottle is connected to the second sample outlet, and an air guide tube is arranged in the raw material storage bottle; the photoreaction container also includes a condensate inlet and a condensate outlet that are connected to the condensation component; The photochemical reaction method also includes: Selecting the non-flow type photoreaction container or the flow type photoreaction container as the photoreaction container for performing a photochemical reaction; When the non-flow type photoreaction container is selected as the photoreaction container for performing the photochemical reaction, the photoreaction container is controlled by the control system to adjust the temperature and gas flow rate for performing the photochemical reaction; When the flow-type photoreaction container is selected as the photoreaction container for photochemical reaction, the photoreaction container is controlled by the control system to adjust the temperature, gas flow rate and photoreaction liquid flow rate for photochemical reaction.