Flow divider, photochemical reaction device and system

Abstract

The utility model relates to the technical field of photochemical reaction equipment, and provides a flow divider, a photochemical reaction device and a photochemical reaction system. The photochemical reaction device comprises an illumination part and a reaction part connected with the illumination part, the illumination part comprises a plurality of illumination modules for providing illumination for the reaction feed liquid; the plurality of illumination modules are enclosed to form an illumination unit; the reaction part comprises a reactor, and a reaction cavity is formed in the reactor; the illumination unit is independent of the reaction cavity, the light-emitting surface of the illumination unit faces the reaction cavity, and an illumination gap is formed between the light-emitting surface and the side wall of the reaction cavity. The illumination unit is formed by enclosing the plurality of illumination modules and is independent from the reaction cavity, and the light-emitting surface of the illumination unit faces the reaction cavity, so that uniform contact of illumination and reaction liquid can be ensured, and the problem that the photochemical reaction efficiency is influenced by the illumination intensity is avoided.

Description

[0001] Cross - reference to related applications

[0002] This utility model claims the priority of a Chinese patent application with the application number 2023110442500 and the publication title "A shunt, a photoreaction device and a system", which was filed on August 17, 2023, and is incorporated herein by reference in its entirety. Technical field

[0003] This utility model relates to the technical field of photoreaction equipment, and particularly relates to a shunt, a photoreaction device and a system. Background art

[0004] Photoreaction is not only applied in organic synthesis, but also can be widely used in other chemical engineering, energy and environmental fields. Currently, existing photoreaction devices basically complete the reaction by irradiating light outside the glassware containing the reaction solution. The light irradiation contacts the reaction solution unevenly and the light irradiation efficiency is low. It is only suitable for micro - scale or semi - medium - scale reactions, and the output in industrial production is limited. Existing photoreaction devices are not suitable for photoreactions with relatively harsh reaction conditions, such as photoreactions with strong acid or strong base reaction media. Summary of the utility model

[0005] In view of at least one problem existing in the prior art, this utility model provides a shunt, a photoreaction device and a system.

[0006] This utility model provides a photoreaction device, comprising:

[0007] A lighting component, including a plurality of lighting modules for providing light to the reaction feed liquid; the plurality of lighting modules enclose to form a lighting unit;

[0008] A reaction component, connected to the lighting component, further including a reactor, and a reaction chamber is formed inside the reactor;

[0009] The lighting unit is independent of the reaction chamber, the light - emitting surface of the lighting unit faces the reaction chamber, and a lighting gap is formed between the lighting unit and the side wall of the reaction chamber.

[0010] In some embodiments, the reaction chamber is sleeved outside the lighting unit. In other embodiments, the lighting unit is sleeved outside the reaction chamber.

[0011] According to the photoreaction device provided by this utility model, the lighting modules are connected in parallel with each other.

[0012] According to the photoreaction device provided by this utility model, the thickness of the lighting gap is 1.0 cm to 4.0 cm, so that the reaction chamber is within a relatively large lighting intensity range of the lighting unit.

[0013] According to the photochemical reaction device provided by the present utility model, the light intensity in the reaction chamber is 5000 μW / cm 2 ~22000 μW / cm 2 .

[0014] According to the photochemical reaction device provided by the present utility model, the light illumination component further includes:

[0015] A limit connection unit, connected to the reaction component, and also detachably and limit-connected to the light illumination module.

[0016] According to the photochemical reaction device provided by the present utility model, the limit connection unit includes:

[0017] A limit plate, covering the end of the light illumination gap; also connected to the reaction component, and a plurality of limit holes arranged circumferentially around the center of the limit plate are spaced on the limit plate; the end of the light illumination module is detachably inserted into the limit holes;

[0018] A connection structure, connected to the limit plate, and also detachably and limit-connected to the light illumination module.

[0019] According to the photochemical reaction device provided by the present utility model, the reaction component further includes:

[0020] A support unit, used for supporting the reactor, and also connected to the light illumination component; the reactor is a coiled pipe.

[0021] According to the photochemical reaction device provided by the present utility model, the photochemical reaction device further includes:

[0022] A cooling component, connected to the light illumination module, and used for cooling the light illumination module.

[0023] According to the photochemical reaction device provided by the present utility model, the light illumination module includes:

[0024] A lamp board;

[0025] A heat dissipation unit, detachably connected to the lamp board, and the heat dissipation units of two adjacent light illumination modules are connected to each other to enclose and form the light illumination unit.

[0026] According to the photochemical reaction device provided by the present utility model, a flow channel is formed inside the heat dissipation unit, and the cooling component is communicated with the flow channel for conveying a cooling medium to the flow channel.

[0027] According to the photochemical reaction device provided by the present utility model, the cooling component includes:

[0028] The diverter has a cavity formed inside. A plurality of diversion openings communicating with the cavity and an inlet / outlet for fluid to flow into or out of the cavity are provided on the side wall of the diverter; each of the diversion openings is communicated with one of the flow channels through a delivery pipe; the distances from each of the diversion openings to the inlet / outlet are the same.

[0029] The photochemical reaction system provided in the second aspect of the present invention further includes the above-mentioned photochemical reaction device, a circulation pump and a power supply;

[0030] The circulation pump is communicated with the reaction component through a material pipe; the power supply is electrically connected to the light irradiation module.

[0031] The present invention also provides a preparation method of an intermediate compound of an etomidate derivative represented by Formula I. The preparation method includes introducing the raw materials required for preparing the intermediate compound of the etomidate derivative into the above-mentioned photochemical reaction device for photochemical reaction to obtain the intermediate compound of the etomidate derivative represented by Formula I;

[0032]

[0033] Formula I

[0034] wherein X and Y are each independently a halogen or hydrogen, provided that X and Y are not both hydrogen; and R 1 is an optionally substituted C 1-6 alkyl, C 2-7 alkoxycarbonyl, C 3-6 cycloalkyl and C 6-10 aryl, with one or more substituents selected from halogen, hydroxyl, amino, cyano, C 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, C 3-6 cycloalkyl or C 6-10 aryl.

[0035] The preparation method of an intermediate compound of an etomidate derivative provided by the present invention satisfies one or more of the following conditions:

[0036] (1) The intermediate compound is a compound represented by Formula II:

[0037]

[0038] Formula II

[0039] Y is selected from F, Cl, Br or I, more preferably F; R 1 is an optionally substituted C 1-6 alkyl, C 2-7 alkoxycarbonyl, C3-6 Cycloalkyl and C 6-10 alkyl substituted with substituents of aryl 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, C 3-6 cycloalkyl or C 6-10 aryl, preferably C 1-6 alkyl, more preferably ethyl;

[0040] (2) The raw material includes the compound shown in Formula III:

[0041]

[0042] Formula III

[0043] In Formula III, R 1 is optionally substituted by one or more substituents selected from halogen, hydroxyl, amino, cyano, C 1-6 alkoxy, C 2-7 alkoxycarbonyl, C 3-6 cycloalkyl and C 6-10 alkyl substituted with substituents of aryl 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, C 3-6 cycloalkyl or C 6-10 aryl, preferably C 1-6 alkyl, more preferably ethyl;

[0044] (3) The raw material includes HBF 4 solution;

[0045] (4) The light intensity in the reaction chamber is 5000 μW / cm 2 ~22000 μW / cm 2 , preferably 10000 μW / cm 2 ~12000 μW / cm 2 ;

[0046] (5) The wavelength of the light emitted by the light-emitting component (1) is 280 - 400 nm, preferably 305 - 310 nm;

[0047] (6) The thickness of the light gap (3) is 1.0 cm - 4.0 cm, preferably 2.0 cm - 4.0 cm, preferably 3.0 cm - 4.0 cm, more preferably 3.5 cm - 4.0 cm.

[0048] The third aspect of the present utility model provides a diverter. A cavity is formed inside the diverter. A plurality of diversion ports communicating with the cavity are provided on the side wall of the diverter, and an inlet / outlet for a cooling medium to flow into or out of the cavity;

[0049] The distance from each of the shunt ports to the inlet / outlet is equal.

[0050] For the flow divider provided by the present utility model, the cavity is a cylindrical cavity, and a plurality of the shunt ports are arranged at intervals around the center of the cavity, and the inlet / outlet is arranged at the center position of the cross-section of the cavity.

[0051] For the flow divider provided by the present utility model, a conveying pipe is inserted into the shunt port, and the on-off valve is arranged on the conveying pipe.

[0052] A flow divider, a photoreaction device and a system provided by the present utility model, by making the lighting unit independent of the reaction chamber, with the light-emitting surface of the lighting unit facing the reaction chamber and being arranged at an interval from the reaction chamber to form a lighting gap, can enable the reaction chamber to be in the area with the maximum lighting intensity of the lighting component, which solves the problem of low lighting efficiency in the prior art, and can enable the light emitted from the light-emitting surface of the lighting unit to uniformly contact the reaction liquid in the reaction chamber, thus solving the problem of uneven contact between the lighting and the reaction liquid in the prior art.

[0053] By enclosing a plurality of lighting modules to form a lighting unit, the total lighting intensity and lighting area of the lighting unit can be adjusted by increasing or decreasing the number of lighting modules. The total lighting intensity of the entire lighting unit can also be adjusted by adjusting the lighting intensity of a single lighting module. Therefore, the reaction efficiency of the photoreaction device of the present utility model is not limited by the lighting intensity, and combined with the fact that the reaction feed liquid can uniformly contact the lighting, the photoreaction device of the present utility model solves the problems of low efficiency and low output in the prior art during industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0054] In order to more clearly illustrate the technical solutions in the present utility model or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present utility model. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0055] Figure 1 is a schematic structural view of a photoreaction device provided by the present utility model under the main visual view.

[0056] Figure 2 is Figure 1 a schematic top view of the photoreaction device shown.

[0057] Figure 3 is Figure 1 a schematic bottom view of the photoreaction device shown.

[0058] Figure 4 is Figure 1 a schematic three-dimensional structure diagram of the illumination component of the photochemical reaction device shown in

[0059] Figure 5 is Figure 4 a schematic structure diagram of the B-B cross-section in the structure shown in

[0060] Figure 6 is Figure 1 a schematic structure diagram of the limit plate of the photochemical reaction device in

[0061] Figure 7 is Figure 1 a schematic structure diagram of the connecting support column of the photochemical reaction device in

[0062] Figure 8 is Figure 1 a schematic assembly structure diagram of the illumination component and the reaction component of the photochemical reaction device shown in

[0063] Figure 9 is Figure 8 a sectional view of the schematic assembly structure diagram shown in the D-D cross-section in

[0064] Figure 10 is Figure 9 a magnified structure diagram at A in the structure shown in

[0065] Figure 11 is the Figure 8 exploded view after exploding the coil pipe and the outer shell in the schematic assembly structure diagram shown in

[0066] Figure 12 is Figure 11 a schematic assembly structure diagram of the support unit and the illumination component in

[0067] Figure 13 is Figure 11 a schematic structure diagram of the illumination module of the illumination component in

[0068] Figure 14 is Figure 13 a magnified structure diagram at F in

[0069] Figure 15 is Figure 13 a magnified structure diagram at G in

[0070] Figure 16 is Figure 1 a schematic structure diagram of the diverter of the photochemical reaction device shown in

[0071] Figure 17 is Figure 16Cross-sectional view of the shunt shown in the E-E section.

[0072] Reference numerals:

[0073] 1. Lighting component; 2. Reaction component; 3. Lighting gap; 4. Cooling component; 5. Support component;

[0074] 11. Lighting module; 12. Lighting unit; 13. Limit connection unit; 21. Reactor; 22. Support unit; 23. Outer shell; 41. Shunt; 42. Switch valve;

[0075] 111. Lamp board; 112. Heat dissipation unit; 131. Limit plate; 132. Connection structure; 221. Support rod; 222. First support plate; 223. Second support plate; 411. Cavity; 412. Shunt port; 413. Inlet / outlet;

[0076] 1121. Flow channel; 1122. Heat dissipation housing; 1123. U-shaped tube; 1124. First ear plate; 1125. Second ear plate; 1311. Limit hole; 1321. Connection plate; 1322. Connection support column;

[0077] 13221. Limit chute. Detailed implementation

[0078] To make the objectives, technical solutions and advantages of the present utility model clearer, the technical solutions in the present utility model will be clearly and completely described below with reference to the accompanying drawings in the present utility model. Obviously, the described embodiments are some, but not all, of the embodiments of the present utility model. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present utility model without making creative efforts fall within the scope of protection of the present utility model.

[0079] "About" in this specification can be understood as within 10%, 9%, 8%, 7%, 6%, 5%, 4%, 3%, 2%, 1%, 0.5%, 0.1%, 0.05% or 0.01% of the stated value. Unless otherwise clearly stated, all numerical values provided herein are modified by the term "about".

[0080] The following combines Figures 1 to 4 , and Figure 9 and Figure 10Describe a photoreaction device of the present utility model. The photoreaction device includes a lighting component 1 and a reaction component 2 connected to the lighting component 1. The lighting component 1 includes a plurality of lighting modules 11 for providing light to the reaction liquid material. The plurality of lighting modules 11 enclose to form a lighting unit 12. The reaction component 2 includes a reactor 21. A reaction chamber for the reaction liquid material to carry out a chemical reaction is formed inside the reactor 21. The lighting unit 12 is independent of the reaction chamber, that is, the lighting unit 12 is outside the reaction chamber. The light-emitting surface of the lighting unit 12 faces the reaction chamber and is spaced apart from the side wall of the reaction chamber to form a lighting gap 3.

[0081] The inventor of the present utility model found that there is an irradiation angle for the light source in the light-emitting surface of the lighting unit 12. Therefore, the relationship between the light intensity of the light-receiving surface and its distance from the light-emitting surface is as follows: when the distance is extremely small, the light intensity of the light-receiving surface does not reach the maximum, but first increases with the increase of the distance. When it increases to the maximum light intensity, the light intensity of the light-receiving surface will decrease with the increase of the distance. Therefore, the lighting unit 12 is arranged independently of the reaction chamber. The light-emitting surface of the lighting unit 12 faces the reaction chamber of the reactor 21 and is spaced apart from the reaction chamber to form a lighting gap 3. In this way, the lighting gap 3 can be set and adjusted so that the reaction chamber of the reactor 21 is in the region with a relatively large light intensity of the lighting component 1. The light passes through the reactor 21 and irradiates the reaction liquid material to initiate a chemical reaction, which can not only ensure the lighting efficiency of the lighting component 1, but also ensure the uniformity of the reaction liquid material in contact with the light. Therefore, the problems of uneven contact between light and reaction liquid material and low lighting efficiency in the prior art are solved.

[0082] Also, because the lighting unit 12 is formed by enclosing a plurality of lighting modules 11, the total lighting intensity and lighting area of the lighting unit 12 can be adjusted by increasing or decreasing the number of lighting modules 11. The total lighting intensity and lighting area of the entire lighting unit 12 can also be adjusted by adjusting the lighting intensity of a single lighting module 11. Therefore, the output of the photoreaction device of the present utility model is not limited by the lighting intensity problem of the lighting unit 12. Combined with the fact that the reaction liquid material can be in uniform contact with the radiation light, the photoreaction device of the present utility model solves the problems of low efficiency and low output in the industrial production process of the existing photoreaction devices.

[0083] In addition, the cross-section of the lighting unit 12 can be an annular shape or a polygon. In the following description, if not otherwise specified, the cross-section of the lighting unit 12 refers to the annular shape, and the annular lighting unit 12 can further improve the uniformity of the reaction liquid material in contact with the light.

[0084] In an embodiment of the present utility model, the illumination unit 12 is independent of the reaction chamber. The light-emitting surface of the illumination unit 12 faces the reaction chamber and is spaced from the side wall of the reaction chamber to form an illumination gap 3, which can be understood as at least two cases:

[0085] In the first case, the illumination unit 12 is sleeved around the periphery of the reaction chamber. That is, the inner side surface of the illumination unit 12 is the light-emitting surface, and the light-emitting surface is sleeved around the periphery of the reaction chamber. Moreover, the outer side wall of the reaction chamber is spaced from the light-emitting surface to form the illumination gap 3.

[0086] In the second case, the reaction chamber is sleeved around the periphery of the illumination unit 12. That is, the outer side surface of the illumination unit 12 is the light-emitting surface, the reaction chamber is sleeved around the light-emitting surface, and the inner side wall of the reaction chamber is spaced from the light-emitting surface to form the illumination gap 3. In the following description of the structure, unless otherwise specified, this case is referred to.

[0087] In some embodiments, the illumination modules 11 are connected in parallel with each other, avoiding the problem that when one illumination module 11 is damaged, the other illumination modules 11 cannot work.

[0088] In order to further ensure uniform contact between the reaction material liquid in the reaction chamber and the illumination, the thickness at each position of the illumination gap 3 is the same, that is, the distance from the light-emitting surface to the side wall of the reaction chamber is equal. In addition, the thickness of the illumination gap 3 is not particularly limited and can be adjusted and set according to the irradiation angle of the light source and the specific arrangement of the light source, etc. But the ultimate goal is to make the reaction chamber of the reactor 21 within the range of the larger illumination intensity of the illumination unit 12.

[0089] In some embodiments, the thickness of the illumination gap 3 is 1.0 cm to 4.0 cm, so that the reaction chamber is within the range of the larger illumination intensity of the illumination unit 12, which can improve the efficiency of the photochemical reaction in the reaction chamber.

[0090] Further, the illumination intensity in the reaction chamber is 5000 μW / cm 2 ~22000 μW / cm 2 . This embodiment can improve the reaction efficiency and yield of a specific photochemical reaction. For example, it can improve the reaction efficiency and yield of the intermediate compound of the etomidate derivative shown in Formula I.

[0091] In a specific photoreaction, the reactor 21 is preferably a continuous reactor, which can improve the production capacity. Moreover, since the reaction feed liquid flows continuously in the reactor, it can also improve the uniform contact between the light and the reaction feed liquid. The reactor 21 can be fed and discharged from above and below; it can also be fed and discharged horizontally. The material of the reactor 21 is glass, ceramic, metal, alloy or Teflon material. When a photoreaction is carried out in the reactor 21, the material of the reactor 21 is glass and Teflon material that can transmit light. When the chemical reaction carried out in the reactor 21 does not require light, the material of the reactor 21 can be either glass and light-transmitting Teflon material, or metal, alloy and light-impermeable Teflon material. When the chemical reaction carried out in the reactor 21 is a light-shielding reaction, the material of the reactor 21 is light-impermeable metal, alloy and light-impermeable Teflon material. In addition, the material of the reactor 21 can also be selected according to the reaction conditions of the chemical reaction. Among them, reactors 21 made of glass, ceramic, metal and alloy are suitable for chemical reactions with relatively mild reaction conditions. For example, they are used for chemical reactions with relatively low corrosivity of the reaction feed liquid. The reactor 21 made of Teflon material is suitable for chemical reactions with relatively harsh reaction conditions. For example, it is suitable for chemical reactions with relatively strong corrosivity of the reaction feed liquid. Among them, Teflon materials include several types such as polytetrafluoroethylene (PTFE), fluorinated ethylene propylene copolymer (FEP), tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer (PFA), ethylene-tetrafluoroethylene copolymer (ETFE), etc. If the chemical reaction in the reaction chamber is a photoreaction, then the material of the reactor 21 is preferably a light-transmitting and / or transparent material, such as tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer (PFA). PFA is also called soluble polytetrafluoroethylene. PFA is light-transmitting, and its physical properties, electrical properties and chemical properties are similar to those of polytetrafluoroethylene. It is a copolymer of a small amount of perfluoropropyl perfluorovinyl ether and polytetrafluoroethylene. Its properties have no change compared with polytetrafluoroethylene. The long-term service temperature is -80°C to 260°C. It has excellent chemical corrosion resistance and is corrosion-resistant to all chemicals. Its friction coefficient is the lowest among plastics, and it also has good electrical properties. Its electrical insulation is not affected by temperature.

[0092] A temperature detection unit and a light intensity detection unit are also provided in the light gap 3. The temperature detection unit and the light intensity detection unit are both connected to the light module 11 and are respectively used to detect the temperature and light intensity of the light module 11. The temperature detection unit can be a temperature sensor, etc., and the light intensity detection unit can be a light intensity detector.

[0093] Next, a specific description of the lighting component 1 will be given.

[0094] In the embodiment of the present utility model, as Figures 4 to 7As shown, the lighting component 1 further includes a limit connection unit 13 connected to the reaction component 2; the limit connection unit 13 is removably and limit-connected to the lighting module 11. By providing the limit connection unit 13, it is convenient to install and disassemble the lighting module 11, facilitating the maintenance of each lighting module 11.

[0095] Furthermore, the limit connection unit 13 includes a limit plate 131 connected to the reaction component 2 and a connection structure 132 connected to the limit plate 131; the limit plate 131 covers the end of the lighting gap 3 to close the lighting gap 3, improving the utilization rate of the light source. A plurality of limit holes 1311 are arranged at intervals on the limit plate 131 and are circumferentially arranged around the center of the limit plate 131. As Figure 6 shown, the end of the lighting module 11 is removably inserted into the limit holes 1311. The cross-section of the lighting unit 12 can be circular. Compared with the polygonal-shaped lighting unit 12, the circular lighting unit 12 can improve the uniformity of the reaction liquid in the reaction chamber receiving light, reduce the probability of the occurrence of photoreaction dead angles, and improve the reaction efficiency. The connection structure 132 is removably and limit-connected to the lighting module 11, facilitating the installation and disassembly of the lighting module 11 and the maintenance of each lighting module 11.

[0096] Preferably, the limit plate 131 is preferably an annular structure, improving the aesthetic appearance of the entire device.

[0097] As Figure 4 shown, the connection structure 132 includes a connection plate 1321 and a plurality of connection support columns 1322; the connection plate 1321 and the limit plate 131 are arranged parallel to each other at intervals; a limit chute 13221 is provided on each connection support column 1322. As Figure 7 shown. One end of each connection support column 1322 is connected to the limit plate 131, and the other end is connected to the connection plate 1321; a plurality of limit chutes 13221 are circumferentially arranged around the center of the limit plate 131, and the side of the lighting module 11 is removably limited in the limit chutes 13221. As Figure 5 shown. This simplifies the installation structure of the entire device, facilitating the installation and disassembly of the lighting module 11 and the maintenance of each lighting module 11.

[0098] The installation process of the lighting module 11: Pass one end of the lighting module 11 through the limit holes 1311, place the side of the lighting module 11 in the limit chutes 13221, and slide along the limit chutes 13221 until the other end of the lighting module 11 is removably inserted into the limit holes 1311, thus completing the installation of the lighting module 11.

[0099] Next, a specific description of the reaction component 2 will be given.

[0100] In the embodiment of the present invention, asFigures 8 to 12 As shown, the reaction component 2 further includes a support unit 22 for supporting the reactor 21; the reactor 21 is a coiled pipe, and the pipe of the coiled pipe is a reaction chamber; the coiled pipe is sleeved around the periphery of the lighting unit 12 and is spaced from the lighting unit 12 to form a lighting gap 3. At this time, the cross-section of the lighting gap 3 is an annular shape. The support unit 22 is also connected to the lighting component 1, as Figure 9 and Figure 10 shown. The feeding and discharging directions of the coiled pipe are horizontal. The horizontal feeding and horizontal discharging design is beneficial to the smooth inlet and outlet of the reaction liquid on the one hand, and is convenient for the formation of the coiled pipe on the other hand. The coiled pipe is formed by winding a pipe around the support unit 22. The size of the pipe is not particularly limited. In some embodiments, the pipe is a pipe with an outer diameter of 12.7 mm and an inner diameter of 9.525 mm. By providing the support unit 22, support can be provided for the reactor 21 so that the coiled pipe is arranged around the periphery of the lighting unit 12 to form a lighting gap 3.

[0101] Furthermore, as Figure 11 and Figure 12 shown, the support unit 22 includes a plurality of support rods 221 connected to the lighting component 1, and a first support plate 222 and a second support plate 223 that are parallel to each other and spaced apart; the plurality of support rods 221 are circumferentially arranged around the center of the lighting unit 12, and each support rod 221 is clamped between the first support plate 222 and the second support plate 223. Specifically: one end of the support rod 221 is connected to the second support plate 223, and the other end passes through the limiting plate 131 and is connected to the first support plate 222 and is connected to the limiting plate 131. The first support plate 222 is also connected to the limiting plate 131. The support rod 221 is spaced from the lighting unit 12; the coiled pipe is wound around the support rod 221. The first support plate 222 and the second support plate 223 respectively cover both ends of the lighting gap 3. Specifically: one end of the lighting gap 3 is closed by the limiting plate 131, and the other end is closed by the second support plate 223. A through hole is opened on the second support plate 223, and the user places detection elements such as a temperature detection unit and a light intensity detection unit in the lighting gap 3 through the through hole. Furthermore, a door for closing the through hole is also installed on the second support plate 223, which can prevent the light in the lighting gap 3 from scattering out of the lighting gap 3.

[0102] For aesthetics, the first support plate 222 and the second support plate 223 are preferably annular structures, and the diameters of the first support plate 222 and the second support plate 223 are not particularly limited. In some embodiments, the diameter of the first support plate 222 is 350 mm to 450 mm, and the diameter of the second support plate 223 is 350 mm to 450 mm. Preferably, the diameters of the first support plate 222 and the second support plate 223 are 400 mm.

[0103] As Figure 8 andFigure 11 As shown, for the need to protect the coiled pipe and for aesthetics, the reaction component 2 further includes a housing 23. The housing 23 is sleeved around the coiled pipe and fits closely with the coiled pipe, and is also connected to the support unit 22. The coiled pipe is sleeved around the periphery of the lighting unit 12. By providing the housing 23, it plays a role in protecting the reactor 21.

[0104] Specifically, the two ends of the housing 23 are respectively connected to the first support plate 222 and the second support plate 223. The housing 23 is preferably made of stainless steel with a thickness of about 2 mm, and the housing 23 also has the function of facilitating the formation of the coiled pipe. When the material of the coiled pipe is PFA, due to the properties of the PFA material itself, the housing 23 facilitates the coiling of the pipe to form a coiled pipe. The height of the housing 23 is not particularly limited. In some embodiments, it is in the range of 500 mm to 600 mm, and in some other embodiments, it is about 541.5 mm. Observation windows (not shown in the figure) are respectively formed at the two ends of the housing 23 along the radial direction and towards the central position. On the one hand, it allows the feed port and the discharge port of the coiled pipe to extend out of the housing, and on the other hand, it facilitates the experimenter to observe the specific reaction situation of the reaction liquid.

[0105] As Figures 1 to 3 shown, since the lighting module 11 will inevitably generate heat during operation, and the heat generation will reduce the service life of the lighting module 11, so the photochemical reaction device of the present utility model further includes a cooling component 4; the cooling component 4 is connected to the lighting module 11 for cooling the lighting module 11. Among them, the cooling component 4 can be a device capable of realizing the cooling function such as a fan, a radiator, a semiconductor refrigeration sheet, a device for cooling with a cooling medium, etc.

[0106] Considering the production cost and use cost of the photochemical reaction device, the cooling component 4 is preferably a device for cooling with a cooling medium. Among them, the cooling medium can be a fluid such as cooling water or cooling gas.

[0107] Next, a specific description of the lighting module 11 will be given.

[0108] In the embodiment of the present utility model, as Figures 13 to 15 shown, the lighting module 11 includes a lamp board 111 and a heat dissipation unit 112; the lamp board 111 is detachably arranged on the heat dissipation unit 112. The heat dissipation units 112 of two adjacent lighting modules 11 are connected to each other to enclose and form a lighting unit 12. By providing the lamp board 111, it can provide an installation basis for installing lamp beads, etc. By providing the heat dissipation unit 112, it can cool the lamp board 111 and the lamp beads, improve the service life of the lamp beads, and improve the service life of the lighting module 11. By detachably connecting the heat dissipation unit 112 to the lamp board, when the lamp board 111 is damaged, the lamp board 111 can be replaced, and the old heat dissipation unit 112 can continue to be equipped for the new lamp board 111, reducing the maintenance cost.

[0109] Further, the lamp board 111 is also connected to a temperature detection unit, which is used to detect the temperature of the lamp board 111 in real time. Each lighting module 11 can be directly connected to an external AC power supply or a DC power supply. The DC power supply is preferably a battery pack, and the battery pack is arranged on the heat dissipation unit 112. Each lighting module 11 is connected in parallel with each other to avoid the problem that when one lighting module 11 is damaged, the other lighting modules 11 cannot work.

[0110] In addition, a lamp is provided on the lamp board 111, and the lamp can be a mercury lamp, an ultraviolet lamp or an LED lamp. LED lamps are classified by wavelength into UVA, UVB, UVC and UVD. Among them, the wavelength of long-wave UVA is between 320 and 400 nanometers, also known as long-wave black spot effect ultraviolet rays. It has strong penetration power and can penetrate glass and even 9 feet of water; and it exists all year round, regardless of sunny or cloudy, morning or evening. Medium-wave UVB, with a wavelength between 275 and 320 nanometers, is also known as medium-wave erythema effect ultraviolet rays. It has medium penetration power. The shorter part of its wavelength will be absorbed by transparent glass, and most of the medium-wave ultraviolet rays contained in sunlight are absorbed by the ozone layer, and only less than 2% can reach the earth's surface, which is particularly strong in summer and afternoon. Short-wave UVC, with a wavelength between 200 and 275 nanometers, is also known as short-wave sterilization ultraviolet rays. It has the weakest penetration ability and cannot penetrate most transparent glass and plastics. Almost all of the short-wave ultraviolet rays contained in sunlight are absorbed by the ozone layer and are absorbed by the ozone layer before reaching the ground. The UVD band has a wavelength of 100-200 nm and is also known as vacuum ultraviolet rays. In some embodiments, the reaction solution undergoes a photochemical reaction, so a UVB LED lamp is preferably used.

[0111] Further, each lighting module 11 includes two lamp boards 111 connected in series. Two mounting grooves are formed on the heat dissipation unit 112, and each lamp board 111 is respectively disposed in the mounting groove, and a temperature detection unit is installed on each lamp board. In some embodiments, there are 198 UVB LED lamps on each lamp board 111. The series-parallel relationship of the 198 UVB LED lamps is as follows: every 11 UVB LED lamps are connected in series to obtain 1 string of UVB LED lamps, and then 18 strings of UVB LED lamps are connected in parallel, which is simply referred to as 11 series and 18 parallel. There are a total of 396 lamp beads on the two lamp boards 111 connected in series, and the series-parallel relationship is: 22 series and 18 parallel. Using two lamp boards 111 can make the illumination more uniform. At the same time, the UVB LED lamp is preferably a dual-chip UVB LED lamp because the dual-chip UVB LED lamp has less self-heating, high photoelectric conversion efficiency, and long service life. When the lighting module 11 is working, the dual-chip UVB LED lamps on each lamp board emit light, but the operating power of a single lighting module 11 can be controlled to be lower than its full-load power, for example, 50%-80% of the full-load power, and in some embodiments, it is about 60%, to improve the service life of the lamp; similarly, the operating power of the entire lighting unit 12 can also be controlled to be lower than its full-load power, for example, 50%-80% of the full-load power, and in some embodiments, it is about 60%, to improve the service life of the lamp. The irradiation angle of the lamp is not particularly limited.

[0112] In some embodiments, the irradiation angle of the lamp is about 60 degrees. In this case, when the lamp board is assembled and emits light, the illumination intensity of the light-receiving surface is more uniform. The size of the lamp board is not particularly limited either. In some embodiments, the size of the lamp board is about 510 mm * 31 mm, and the UVB LED lamps are evenly spaced. The distance between the lamps on the lamp board 111 and the inner side wall of the coil is set according to the irradiation angle of the light source, the specific arrangement of the light source, etc. This distance can make the reaction chamber of the reactor 21 within the range of the larger illumination intensity of the lighting unit 12.

[0113] In some embodiments, this distance is within the range of 1.0 cm to 4.0 cm. In other embodiments, considering the convenience of observation, maintenance, detection, etc., this distance is within the range of 2.0 cm to 4.0 cm, or within the range of 3.0 cm to 4.0 cm, or within the range of 3.5 cm to 4.0 cm.

[0114] Next, the heat dissipation unit 112 and the cooling component 4 will be specifically described.

[0115] When the cooling component 4 cools the lighting module 11 by using a cooling medium, such as Figure 5As shown, a flow channel 1121 is formed on the heat dissipation unit 112, and the cooling component 4 is communicated with the flow channel 1121 for conveying a cooling medium to the flow channel 1121. By providing the flow channel 1121 in the heat dissipation unit 112, the heat dissipation efficiency can be improved.

[0116] As Figures 13 to 15 shown, the heat dissipation unit 112 includes a heat dissipation housing 1122, a U-shaped tube 1123, a first ear plate 1124, and a second ear plate 1125. A plurality of flow channels 1121 are formed in the heat dissipation housing 1122. The number of U-shaped tubes 1123 is at least one, and each U-shaped tube 1123 is communicated with two flow channels 1121 to form a circulation channel. Two ends of the heat dissipation housing 1122 are respectively connected to the first ear plate 1124 and the second ear plate 1125, wherein the first ear plate 1124 is located on the side where the lamp board 111 is assembled; the second ear plate 1125 is located on the other side opposite to the side where the lamp board 111 is assembled. The side wall of the heat dissipation housing 1122 is detachably limited in the limiting chute 13221. During the assembly process, while the first ear plate 1124 is detachably inserted and limited in the limiting hole 1311, the side wall of the heat dissipation housing 1122 is detachably limited and installed in the limiting chute 13221, which facilitates the disassembly and installation of a single light illumination module 11.

[0117] A through hole is formed on the second ear plate 1125, and a cable is passed through the through hole, which can make the appearance of the photochemical reaction device more tidy and beautiful. The power supply, the male-female docking connector, and the lamp board 111 are connected by a cable. Using the male-female docking connector is convenient for installation and realizes quick connection and disconnection. Of course, the connection between the power supply and the lamp board 111 is not limited to using the male-female docking plug, and other electrical connection methods can also be used as long as the lamp board 111 can be powered. In a specific embodiment, the number of flow channels 1121 is two, and the U-shaped tube 1123 is connected to the ends of the two flow channels 1121 to form a circulation channel, and the inlet and outlet of the circulation channel are both at the same end of the heat dissipation housing 1122. In this way, the same end for entering and discharging the cooling medium can make the heat dissipation more uniform, and the cooling medium in the flow channel 1121 can be prevented from overflowing during disassembly.

[0118] As Figure 16 and Figure 17 shown, the cooling component 4 includes a flow divider 41; a cavity 411 is formed inside the flow divider 41, a plurality of flow dividing ports 412 are formed on the side wall of the flow divider 41, and an inlet / outlet 413 for the cooling medium to flow into or out of the cavity 411; each flow dividing port 412 communicates the cavity 411 with a flow channel 1121 through a conveying pipe; and the distance from each flow dividing port 412 to the inlet / outlet 413 is the same. Such a design can ensure that the cooling medium in the cavity 411 enters the flow dividing ports 412 at the same time and has the same flow rate.

[0119] Further, the cavity 411 is a cylindrical cavity, and a plurality of shunt ports 412 are arranged at intervals around the center of the cavity 411. The inlet / outlet 413 is provided at the center position of the cross-section of the cavity 411. The flow rates of the cooling medium that can enter the plurality of shunts 412 simultaneously are equal.

[0120] Further, in order to control the flow rate of the cooling medium passing through the shunt port 412, the cooling component 4 of the present utility model further includes a switching valve 42. The switching valve 42 is arranged on the delivery pipe to control the flow rate of the cooling medium flowing through the shunt port 412. The switching valve 42 can be a manual regulating valve, an electromagnetic valve or an electric regulating valve. The position of the cooling component 4 relative to the lighting component 1 is not limited.

[0121] In an embodiment of the utility model, the number of the shunt devices 41 is two. The shunt port 412 of one shunt device 41 is communicated with the inlet of the flow channel 1121 through a delivery pipe; the shunt port 412 of the other shunt device 41 is communicated with the outlet of the flow channel 1121 through a delivery pipe. The external cooling medium (such as cooling water) sequentially passes through the inlet / outlet 413 of the first shunt device 41, the cavity 411 of the first shunt device 41, the shunt port 412 of the first shunt device 41, the delivery pipe, the inlet of the flow channel 1121, the flow channel 1121, the outlet of the flow channel 1121, the delivery pipe, the shunt port 412 of the second shunt device 41, the cavity 411 of the second shunt device 41 and the inlet / outlet 413 of the second shunt device 41 to complete the cooling of the lighting module 11. The positions of the two shunt devices 41 are not limited in the present utility model. However, considering safety, the cooling component 4 is installed below the lighting module 11, so as to avoid the problem that the cooling medium of the cooling component 4 drips onto the lighting module 11 and damages the lighting module 11.

[0122] In an embodiment of the present utility model, the photoreaction device further includes a support component 5; the support component 5 is connected to both the lighting component 1 and the reaction component 2, and the reaction component 2 is arranged on the support component 5 in a vertical or horizontal manner. The support component 5 includes a plurality of support legs. The top of each support leg forms a frustum, and a rubber pad is provided at the bottom of each support leg. The height of the support legs is not particularly limited. In some embodiments, it is in the range of 450 mm to 550 mm, and in some other embodiments, it is about 496 mm.

[0123] When the reaction component 2 is arranged on the support component 5 in a vertical manner, as Figure 1As shown, the number of support legs is at least three, and the three support legs are evenly arranged at circumferential intervals along the center of the first support plate 222. The first support plate 222 is horizontally placed on the platform and fixedly connected to each support leg. In this way, it is ensured that the reaction component 2 and the lighting component 1 are stably arranged in a vertical state on the support component 5. At this time, the diverter 41 of the cooling component 4 is arranged below the reaction component 2 and the lighting component 1 and is located between multiple support legs and fixedly connected to the support legs.

[0124] When the reaction component 2 is arranged horizontally on the support component 5, the number of support legs is at least two, and the two support legs are arranged at radial intervals along the outer shell 23. The outer shell 23 is placed on the platform of the support legs.

[0125] The present utility model also provides a photoreaction system, including the photoreaction device, circulation pump and power supply in any of the above embodiments. The circulation pump is communicated with the reaction component 2 through a material pipe; the power supply is electrically connected to the lighting module 11. After adding the reaction feed liquid into the reaction component 2, the reaction component 2 is communicated with the circulation pump through the material pipe. According to the requirement of the photoreaction for the illumination intensity, the lamp of the lighting module 11 is turned on, and the circulation pump is started to make the reaction feed liquid circulate in the reaction cavity of the reactor 21. In this way, it can make the lighting module 11 irradiate the reaction feed liquid more evenly, improving the reaction efficiency and conversion rate of the photoreaction.

[0126] The present utility model also provides a preparation method of an intermediate compound of an etomidate derivative shown in Formula I. The preparation method includes introducing the raw materials required for preparing the intermediate compound of the etomidate derivative into the photoreaction device in any of the above embodiments for photoreaction to obtain the intermediate compound of the etomidate derivative shown in Formula I;

[0127]

[0128] Formula I

[0129] Wherein, X and Y are each independently halogen or hydrogen, provided that X and Y are not simultaneously hydrogen; and R 1 is optionally substituted by one or more substituents selected from halogen, hydroxyl, amino, cyano, C 1-6 alkoxy, C 2-7 alkoxycarbonyl, C 3-6 cycloalkyl and C 6-10 aryl-substituted C 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, C 3-6 cycloalkyl or C 6-10 aryl.

[0130] By using the photochemical reaction device of any of the above embodiments, the intermediate compound of the etomidate derivative shown in Formula I can be prepared, and the reaction efficiency and yield of the intermediate compound of the etomidate derivative shown in Formula I can be improved.

[0131] Specifically, R 1 is selected from C 1-6 alkyl substituted by a substituent, substituted C 2-6 alkenyl, substituted C 2-6 alkynyl, substituted C 3-6 cycloalkyl or substituted C 6-10 aryl; wherein the substituent is selected from at least one of halogen, hydroxyl, amino, cyano, C 1-6 alkoxy, C 2-7 alkoxycarbonyl, C 3-6 cycloalkyl or C 6-10 aryl.

[0132] In some embodiments, the intermediate compound is the compound shown in Formula II. In some embodiments, Y is selected from F, Cl, Br or I, more preferably F. In some embodiments, R 1 is optionally substituted by one or more substituents selected from halogen, hydroxyl, amino, cyano, C 1-6 alkoxy, C 2-7 alkoxycarbonyl, C 3-6 cycloalkyl and C 6-10 aryl substituted C 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, C 3-6 cycloalkyl or C 6-10 aryl, preferably substituted C 1-6 alkyl, more preferably substituted ethyl. In some embodiments, Y is F and R 1 is substituted ethyl.

[0133]

[0134] Formula II.

[0135] In some embodiments, the raw material includes the compound shown in Formula III. In some embodiments, R 1 in Formula III is as defined in the previous Formula I and / or Formula II.

[0136]

[0137] Formula III.

[0138] In some embodiments, the raw material includes HBF 4 solution.

[0139] In some embodiments, the light intensity in the reaction chamber is 5000 μW / cm 2 ~22000 μW / cm 2 and preferably 10000 μW / cm 2 ~12000 μW / cm 2 .

[0140] In some embodiments, the wavelength of the light emitted by the light component 1 is 280 - 400 nm, preferably 305 - 310 nm.

[0141] In some embodiments, the thickness of the light gap 3 is 1.0 cm to 4.0 cm, preferably 2.0 cm to 4.0 cm, more preferably 3.0 cm to 4.0 cm, and even more preferably 3.5 cm to 4.0 cm.

[0142] In this embodiment, by limiting the types of raw materials, the light intensity in the reaction chamber, the thickness of the light gap 3, and the wavelength of the light, the reaction efficiency and the yield can be further improved.

[0143] In a specific embodiment, taking the preparation of ethyl 4 - fluoro - 1 H -imidazole - 5 - carboxylate as an example: Under an ice bath, dissolve ethyl 4 - amino - 1 H -imidazole - 5 - carboxylate in a 50% HBF4 solution, add an aqueous solution containing NaNO 2 to obtain a reaction feed liquid; start the circulation pump, add the reaction feed liquid into the reaction chamber of the reactor 21, that is, into the coiled pipe, the thickness of the light gap 3 is 3.5 cm to 4.0 cm, turn on the lamp of the light module 11, the wavelength of the light emitted by the light module 11 is 305 - 310 nm, and adjust the light intensity so that the light intensity in the reaction chamber is within the range of 10000 μW / cm 2 ~12000 μW / cm 2 , with an average light intensity of 11300 μW / cm 2 , continuously irradiate the reaction feed liquid, collect the reaction liquid from the outlet of the reactor, and perform post - treatments such as separation and concentration on it to obtain colorless oily ethyl 4 - fluoro - 1 H -imidazole - 5 - carboxylate.

[0144] The present utility model also provides a diverter, as shown in Figure 16 and Figure 17 , an inner cavity 411 is formed inside the diverter, a plurality of diversion ports 412 communicating with the cavity 411 are provided on the side wall of the diverter, and an inlet / outlet 413 for the cooling medium to flow into or out of the cavity 411; the distance from each diversion port 412 to the inlet / outlet 413 is equal, so as to ensure that the cooling medium entering the cavity 411 can flow towards the diversion ports 412 at the same time and with the same flow rate.

[0145] Furthermore, the cavity 411 is a cylindrical cavity, and a plurality of shunt ports 412 are arranged at intervals around the center of the cavity 411. The inlet / outlet 413 is provided at the center position of the cross-section of the cavity 411, so as to ensure that the distances from the inlet / outlet 413 to each shunt port 412 are equal.

[0146] In addition, in order to control the flow rate of the cooling medium passing through the shunt port 412, a switching valve 42 is further provided on the delivery pipe installed in the shunt port 412. The switching valve 42 can be a manual regulating valve, an electromagnetic valve or an electric regulating valve.

[0147] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A photochemical reaction device, characterized in that: include: An illumination component (1) comprises a plurality of illumination modules (11) for providing illumination to a reaction liquid; the plurality of illumination modules (11) are enclosed to form an illumination unit (12); A reaction component (2) is connected to the illumination component (1), and further comprises a reactor (21), wherein a reaction chamber is formed in the reactor (21); The illumination unit (12) is independent of the reaction chamber; a light-emitting surface of the illumination unit (12) faces the reaction chamber, and an illumination gap (3) is formed between the illumination unit (12) and a side wall of the reaction chamber.

2. The photochemical reaction device according to claim 1, characterized in that: The illumination modules (11) are connected in parallel with each other.

3. The photochemical reaction device according to claim 1, characterized in that: The thickness of the illumination gap (3) is 1.0 cm to 4.0 cm, so that the reaction chamber is within a larger illumination intensity range of the illumination unit (12).

4. The photochemical reaction device according to claim 3, characterized in that: The light intensity in the reaction chamber is 5000 μW / cm 2 ~22000μW / cm 2 .

5. The photochemical reaction device according to claim 1, characterized in that: The illumination component (1) further comprises: The limiting connection unit (13) is connected to the reaction component (2) and is also connected to the illumination module (11) in a limiting and detachable manner.

6. The photochemical reaction device according to claim 5, characterized in that: The limiting connection unit (13) comprises: A limit plate (131) is arranged to cover the end of the illumination gap (3); it is also connected to the reaction component (2); a plurality of limit holes (1311) are arranged at intervals on the limit plate (131) and are arranged circumferentially around the center of the limit plate (131); the end of the illumination module (11) is detachably inserted into the limit hole (1311); The connection structure (132) is connected to the limiting plate (131) and is also detachably connected to the illumination module (11) in a limiting manner.

7. The photochemical reaction device according to claim 1, characterized in that: The reaction chamber is sleeved on the periphery of the illumination unit (12).

8. The photochemical reaction device according to any one of claims 1 to 7, characterized in that: The reaction component (2) further comprises: A support unit (22) is used to support the reactor (21) and is also connected to the illumination component (1); the reactor (21) is a coil.

9. The photochemical reaction device according to claim 8, characterized in that: The photochemical reaction device also includes: A cooling component (4) is connected to the illumination module (11) and is used to cool the illumination module (11).

10. The photochemical reaction device according to claim 9, characterized in that: The illumination module (11) comprises: Light board (111); The heat dissipation unit (112) is detachably connected to the light panel (111), and the heat dissipation units (112) of two adjacent illumination modules (11) are interconnected to enclose the illumination unit (12).

11. The photochemical reaction device according to claim 10, characterized in that: A flow channel (1121) is formed inside the heat dissipation unit (112), and the cooling component (4) is in communication with the flow channel (1121) and is used to transport cooling medium to the flow channel (1121).

12. The photochemical reaction device according to claim 11, characterized in that: The cooling component (4) comprises: A flow divider (41) is formed with a cavity (411) therein; a plurality of flow dividers (412) in communication with the cavity (411) and an inlet / outlet (413) for fluid to flow into or out of the cavity (411) are formed on a side wall of the flow divider (41); each of the flow dividers (412) is in communication with one of the flow channels (1121) via a delivery pipe; and the distances from each of the flow dividers (412) to the inlet / outlet (413) are the same.

13. A photochemical reaction system, characterized in that: A photochemical reaction device comprising any one of claims 1 to 12, a circulation pump and a power supply; The circulation pump is connected to the reaction component (2) via a material pipe; and the power supply is electrically connected to the illumination module (11).

14. A flow divider, characterized in that: A cavity (411) is formed inside the flow divider (41), and a side wall of the flow divider (41) is provided with a plurality of flow diversion ports (412) in communication with the cavity (411), and an inlet / outlet port (413) for fluid to flow into or out of the cavity (411); The distance between each of the branch ports (412) and the inlet / outlet (413) is equal.

15. The flow divider according to claim 14, characterized in that The cavity (411) is a cylindrical cavity, a plurality of the diversion ports (412) are arranged at intervals around the center of the cavity (411), and the inlet / outlet (413) is located at the center of the cross section of the cavity (411).

16. The flow divider according to claim 15, characterized in that A delivery pipe is installed in the diversion port (412), and a switch valve (42) is arranged on the delivery pipe.

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