Flow type chemical reaction device for photoreaction

Abstract

The utility model provides a flow type chemical reaction device for photoreaction, which relates to the technical field of photochemical experiments and comprises a reactor, the reactor comprises a shell, a light-transmitting tube, a light source component and a heat dissipation component, a supporting structure is arranged in the shell, the light-transmitting tube is wound on the periphery of the supporting structure, a liquid flow channel is formed in the light-transmitting tube, and the light source component is arranged in the liquid flow channel. The two ends of the light-transmitting tube extend out of the shell and form an inlet and an outlet respectively, the light source component is arranged on the inner side of the side wall of the shell, and the heat dissipation component is arranged on the inner side of the top wall of the shell. The problems that in the prior art, it is difficult to ensure that reactants at all positions receive light consistently, and temperature rise is difficult to control are solved.

Description

TECHNICAL FIELD

[0001] The utility model belongs to photochemical experiment technical field, more specifically, relate to a flow type chemical reaction device for photo reaction. BACKGROUND

[0002] The rapid development of modern organic photochemical synthesis started in 2008 when Professor MacMillan of Princeton University innovatively combined photocatalysis with secondary amine catalysis, achieving asymmetric alpha-alkylation of aldehyde compounds. In the following decade, photochemical synthesis methods have become an important part of the field of organic catalytic synthesis due to their high efficiency, mildness, environmental friendliness, and other characteristics, and have been widely used in many fields such as material science and biomedical science. However, there are still challenges in its large-scale application.

[0003] Firstly, small-scale photo reactors usually use point light sources or parallel light, which is difficult to ensure that all reactants are inhibited by light when the reaction scale is enlarged, thereby affecting the reaction effect and reaction efficiency. Secondly, the commonly used point light source or parallel light source itself will heat up, and the light source irradiation of the reaction liquid will cause the temperature of the reaction system to rise, plus the reaction itself will release a certain amount of heat, with the increase of the reaction scale, these heat is usually unable to be effectively released, thereby affecting the reaction stability and reaction efficiency. SUMMARY

[0004] The utility model aims at the deficiency existing in the prior art, provides a flow type chemical reaction device for photo reaction, solves the problem that the photo reactor in the prior art is difficult to ensure that all reactants are uniformly inhibited by light and difficult to control temperature rise.

[0005] In order to realize the above-mentioned purpose, the utility model provides a flow type chemical reaction device for photo reaction, which comprises:

[0006] The reactor comprises a shell, a light-transmitting tube, a light source component and a heat dissipation component, the inside of the shell is provided with a support structure, the light-transmitting tube is wound around the outer periphery of the support structure, the inside of the light-transmitting tube forms a liquid flow channel, the two ends of the light-transmitting tube extend to the outside of the shell and form an inlet and an outlet respectively, the light source component is arranged on the inner side of the side wall of the shell, and the heat dissipation component is arranged on the inner side of the top wall of the shell.

[0007] Optionally, the shell comprises a base and a cover body, and the support structure comprises a vertically extending cylindrical component arranged on the upper side of the base.

[0008] Optionally, the light-transmitting tube is spirally wound around the outer periphery of the cylindrical component, and the pitch is uniform.

[0009] Optionally, the light source component comprises a plurality of light emitting elements, and the plurality of light emitting elements are uniformly distributed on the inner side of the side wall of the cover body in a circumferential direction to form a ring-shaped light emitting body.

[0010] Optionally, the ring-shaped light emitting body is provided with at least two along the axial direction of the cover body.

[0011] Optionally, the heat dissipation component comprises a fan, and an air outlet of the fan is arranged downward.

[0012] Optionally, the base is disc-shaped, and the side wall of the cover body is cylindrical.

[0013] Optionally, the inlet is connected with a raw material container through a raw material conveying component, and the outlet is connected with a product receiving container.

[0014] Optionally, the shell is provided with a ventilation opening.

[0015] Optionally, the material of the shell is plastic.

[0016] The utility model provides a kind of flow chemical reaction device for photo reaction, its beneficial effect is at: the flow chemical reaction device for photo reaction is provided with support structure in the shell of reactor, and light transmission pipe is wound in the outer periphery of support structure, and light source component is provided with in the inner side of the side wall of shell, and light is provided, and the liquid flow passage inside light transmission pipe is used to supply reaction liquid reaction and flow, the setting of light transmission pipe forms large surface area-volume ratio, increases the light receiving area of reaction liquid and makes it light evenly, simultaneously, heat dissipation component is arranged in the inner side of the top wall of shell, and help reactor inside and reaction liquid are cooled, to avoid temperature rise too high.

[0017] Other features and advantages of the utility model will be described in detail in the following specific embodiment part. BRIEF DESCRIPTION OF DRAWINGS

[0018] The above and other objects, features and advantages of the present utility model will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings, in which like reference characters refer to like parts throughout the several views, and in which the exemplary embodiments of the present utility model are shown.

[0019] Figure 1 The structure diagram of a kind of flow chemical reaction device for photo reaction according to one embodiment of the utility model is shown.

[0020] Mark explanation:

[0021] 1, reactor; 2, light-transmitting tube; 3, light source component; 4, heat dissipation component; 5, support structure; 6, base; 7, cover; 8, raw material container; 9, raw material conveying component; 10, product receiving container. DETAILED DESCRIPTION

[0022] The preferred embodiments of the present application will be described in more detail below. Although the preferred embodiments of the present application are described below, it is understood that the present application can be implemented in various forms and should not be limited by the embodiments set forth herein. On the contrary, these embodiments are provided so that the present application is more thorough and complete, and the scope of the present application is fully conveyed to those skilled in the art.

[0023] As shown in Figure 1 The present application provides a flow-type chemical reaction device for photo-reaction, comprising:

[0024] The reactor 1 comprises a shell, a light-transmitting tube 2, a light source component 3 and a heat dissipation component 4. The inside of the shell is provided with a support structure 5. The light-transmitting tube 2 is wound around the outer periphery of the support structure 5. The inside of the light-transmitting tube 2 forms a liquid flow channel. The two ends of the light-transmitting tube 2 extend to the outside of the shell and form an inlet and an outlet, respectively. The light source component 3 is arranged on the inner side of the side wall of the shell. The heat dissipation component 4 is arranged on the inner side of the top wall of the shell.

[0025] Specifically, to solve the problem that the light reactor 1 in the prior art cannot ensure that the reactants are uniformly illuminated everywhere and cannot control the temperature rise; the flow-type chemical reaction device for photo-reaction provided by the present application is provided with a support structure 5 in the shell of the reactor 1. The light-transmitting tube 2 is wound around the outer periphery of the support structure 5. The light source component 3 arranged on the inner side of the side wall of the shell provides illumination. The liquid flow channel in the light-transmitting tube 2 is used for reaction and flow of the reaction liquid. The arrangement of the light-transmitting tube 2 forms a large surface area-volume ratio, which increases the light receiving area of the reaction liquid and makes it uniformly illuminated. At the same time, the heat dissipation component 4 arranged on the inner side of the top wall of the shell helps to dissipate heat inside the reactor 1 and the reaction liquid, avoiding excessive temperature rise.

[0026] Optionally, the shell comprises a base 6 and a cover 7. The support structure 5 comprises a vertically extending cylindrical component arranged on the upper side of the base 6.

[0027] Specifically, the base 6 can be disc-shaped. The cover 7 can be detachably connected to the upper side of the base 6. The support structure 5 is arranged at the central position on the upper side of the base 6, so that the light-transmitting tube 2 wound thereon is as centered as possible in the shell.

[0028] Further, the shell is provided with an opening. The light-transmitting tube 2 passes through the opening and extends outwardly.

[0029] In the embodiment, one opening is provided on the lower end of the cover 7, and both ends of the light-transmitting tube 2 pass through the opening, so that the inlet and outlet are both extended downward.

[0030] Optionally, the light-transmitting tube 2 is spirally wound on the outer periphery of the cylindrical component, and the pitches are uniform.

[0031] Specifically, the light-transmitting tube 2 is wound on the cylindrical component for multiple turns to form multiple liquid flow channels of the reaction liquid which are nearly parallel, and the uniform pitches can further improve the consistency of light receiving.

[0032] In the embodiment, the light-transmitting tube 2 is tightly contacted between each turn wound on the outer periphery of the cylindrical component.

[0033] Optionally, the light source component 3 includes multiple light-emitting elements which are uniformly distributed on the inner side of the side wall of the cover 7 in the circumferential direction to form a ring-shaped light-emitting body.

[0034] Specifically, the light-emitting elements are common ultraviolet or visible light sources, and the uniform distribution of the multiple light-emitting elements in the circumferential direction can make the light receiving of one turn of the light-transmitting tube 2 more uniform, further improving the consistency of light receiving.

[0035] Optionally, the ring-shaped light-emitting body is arranged at least two in the axial direction of the cover 7.

[0036] Specifically, the uniform arrangement of the ring-shaped light-emitting body in the vertical direction makes the light distribution in the vertical direction more uniform.

[0037] In the embodiment, the ring-shaped light-emitting body is arranged three in the axial direction of the cover 7, and the vertical height of the ring-shaped light-emitting body on the inner side of the side wall of the cover 7 is matched with the winding height of the light-transmitting tube 2 on the support structure 5, so that the light distribution in the vertical direction also has good consistency.

[0038] Optionally, the heat dissipation component 4 includes a fan, and the air outlet of the fan is arranged downward.

[0039] Specifically, the fan blows air downward from the top of the housing to dissipate heat for the inside of the reactor 1 and the reaction liquid.

[0040] Optionally, the base 6 is disc-shaped, and the side wall of the cover 7 is cylindrical.

[0041] Specifically, the design of the housing which is circular in plan view, in combination with the cylindrical component which is coaxially arranged on the upper side of the base 6, can make the distance between the light-transmitting tube 2 and the light source component 3 consistent.

[0042] In the embodiment, the base 6 and the cover 7 are detachably connected, the outer periphery of the base 6 is provided with an annular groove, and the bottom end of the cover 7 can be embedded in the groove and connected with the base 6.

[0043] Optionally, the raw material container 8, the raw material conveying component 9 and the product receiving container 10 are further included, the inlet is connected with the raw material container 8 through the raw material conveying component 9, and the outlet is connected with the product receiving container 10.

[0044] Specifically, the raw material container 8, the raw material conveying component 9, the reactor 1 and the product receiving container 10 are sequentially connected, the reaction solution in the raw material container 8 is input into the light-transmitting tube 2 inside the reactor 1 through the inlet of the raw material conveying component 9, flows out through the outlet after photochemical reaction and enters the product receiving container 10, the light required for the reaction is provided by the light source component 3 located on the inner side of the side wall of the shell, and the fan located on the inner side of the top wall of the shell cools and reduces the temperature inside the whole reactor 1.

[0045] In the embodiment, the raw material container 8, the raw material conveying component 9 and the product receiving container 10 are respectively a raw material bottle, a peristaltic pump and a product receiving bottle.

[0046] Optionally, the shell is provided with a ventilation opening.

[0047] Specifically, the ventilation opening can be arranged at the upper end and / or the lower end of the shell, so that the inside of the shell is conveniently ventilated and cooled, and the operation of the fan can achieve good cooling effect.

[0048] Optionally, the material of the shell is plastic.

[0049] Specifically, the base 6 and the cover 7 can be made of plastic material, and the cylindrical component can be integrally formed with the base 6.

[0050] In summary, the flow type chemical reaction device for photo reaction provided by the utility model is simple in structure and easy to operate, can be applied to undergraduate experimental teaching, can effectively expand the opening range of the present stage undergraduate organic chemistry teaching experiment, and enables students to understand the research hotspots and new synthesis technologies of the subject frontiers. Taking the use in one teaching as an example: based on the flow type chemical reaction device for photo reaction, the present experiment takes the photochemical synthesis of herbicide bisphenylaminobenmide as the guide, combines organic photochemistry and continuous flow chemistry and applies to undergraduate experimental teaching, and the synthetic chemical formula is as follows.

[0051]

[0052] The present experiment realizes the green synthesis of bisphenylaminobenmide through the continuous flow reaction of the flow type chemical reaction device for photo reaction, generates a high-activity enone intermediate through Wolff rearrangement reaction under the irradiation of a blue lamp as a light source by taking 2-diazo-1,2-diphenyl ethanone as a raw material, then the nucleophilic addition reaction of dimethylamine is performed, and the target product is obtained at a yield of 60%. The preparation method is as follows:

[0053] Take 5 mL 1,2-dichloroethane in a small conical flask, rinse the continuous flow reactor 1 pipeline, adjust the flow rate to 30-40 r·min -1 After the solvent completely enters the reactor 1, increase the inlet, suck air through the inlet to discharge the liquid in the light tube 2, wait for the pipeline to be empty of the solvent. At the same time, add 1.1 g of phenyl benzoyl diazomethane, 1,2-dichloroethane, 10 equivalents of dimethylamine and a magnetic stirrer to a 100 mL dry round-bottom flask and shake to mix uniformly. Then replace the small conical flask with the round-bottom flask containing the reaction solution, and adjust the flow rate to 15 r·min -1 Pump into the flow chemical reaction device for photo-reaction, start the light source part 3 and the heat dissipation part 4, and fully react. During the process, the reaction solution flows in the whole device and receives light. During the reaction, the reaction progress is monitored by TLC (V 石油醚 ∶V 乙酸乙酯 = 5:1), and the reaction is completed in 40-60 minutes. When the reaction is completed, take 5 mL 1,2-dichloroethane in a small conical flask, rinse the light tube 2 again, and adjust the flow rate to 30-40 r·min -1 After rinsing, combine the rinse solution. Column chromatography is performed with V 石油醚 / V 乙酸乙酯 = 5:1-2:1 to directly obtain the target product in the form of white powdery solid, weigh and calculate the yield.

[0054] The above has described various embodiments of the present application, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes are obvious to those skilled in the art without departing from the scope and spirit of the described embodiments.

Claims

1. A flow chemical reaction apparatus for photoreaction, characterized by, The application relates to a reactor, which comprises a shell, a light-transmitting tube, a light source component and a heat dissipation component, the inside of the shell is provided with a support structure, the light-transmitting tube is wound around the outer periphery of the support structure, the inside of the light-transmitting tube forms a liquid flow channel, the two ends of the light-transmitting tube extend to the outside of the shell and form an inlet and an outlet respectively, the light source component is arranged on the inner side of the side wall of the shell, and the heat dissipation component is arranged on the inner side of the top wall of the shell. The shell comprises a base and a cover body, and the support structure comprises a vertically-extended cylindrical component arranged on the upper side of the base.

2. The flow chemical reactor for photo-reaction according to claim 1, wherein The light-transmitting tube is spirally wound around the outer periphery of the cylindrical component, and the pitch is uniform.

3. The flow chemical reactor for photoreaction according to claim 2, wherein The light source component comprises a plurality of light-emitting elements, and the plurality of light-emitting elements are uniformly distributed on the inner side of the side wall of the cover body in the circumferential direction to form a ring-shaped distributed light-emitting body.

4. The flow chemical reactor for photoreaction according to claim 2, wherein The ring-shaped distributed light-emitting body is arranged at least two in the axial direction of the cover body.

5. The flow chemical reactor for photoreaction according to claim 4, wherein The heat dissipation component comprises a fan, and the air outlet of the fan is arranged downward.

6. The flow chemical reactor for photoreaction according to claim 1, wherein The base is disc-shaped, and the side wall of the cover body is cylindrical.

7. The flow chemical reactor for photoreaction according to claim 2, wherein The reactor further comprises a raw material container, a raw material conveying component and a product receiving container, the inlet is connected with the raw material container through the raw material conveying component, and the outlet is connected with the product receiving container.

8. The flow chemical reactor for photoreaction according to claim 1, wherein The shell is provided with a ventilation opening.

9. The flow chemical reactor for photoreaction according to claim 1, wherein The material of the shell is plastic.

10. The flow chemical reactor for photoreaction according to claim 1, wherein ​

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