Continuous flow photoelectrocatalysis reaction instrument

Abstract

The invention relates to the technical field of photoelectrocatalysis synthesis, and discloses a continuous flow photoelectrocatalysis reaction instrument which is high in reaction rate and reliability and comprises a photoelectrocatalysis reaction module and an illumination module. The photoelectrocatalysis reaction module is formed by laminating a lower box body, an anode plate, a runner sheet, a cathode plate, optical glass and an upper cover; a runner joint is arranged on one side of the lower box body and is used for inputting and outputting reaction fluid; a detachable power supply mechanism is arranged on the side wall of the lower box body to supply power to the photoelectric catalytic reaction module; runner sheets are arranged on the upper end face and the lower end face of the anode plate, runners consistent with the runner sheets are formed in the anode plate, the upper cover is of a middle hollow structure, and light is received through optical glass to form a light path; the illumination module is used for providing a light source for the photoelectrocatalysis reaction module; the anode plate and the cathode plate are made of non-photosensitive electrodes, so that a light source generated by the illumination module is prevented from being absorbed by the anode plate and the cathode plate, and the light source can fully act on the fluid to be reacted.

Description

Technical Field

[0001] The invention relates to the technical field of photoelectrocatalytic synthesis, and more specifically to a continuous flow photoelectrocatalytic reactor. Background Art

[0002] The technical field of the present invention is photoelectrocatalysis, which is a synergistic system combining photocatalysis and electrochemistry. Photoelectrocatalysis is divided into two categories, one is photoelectrocatalysis based on photosensitive electrodes, and the other is molecular photoelectrocatalysis based on molecular light-absorbing species. After absorbing the light source, the photosensitive electrode can generate voltage, which is the traditional photoelectrocatalytic method. Molecular photoelectrocatalysis is an emerging research direction. Instead of using photosensitive electrodes, molecules in the solution are used as light-absorbing substances. At present, molecular photoelectrocatalytic reactions mainly use bottle-type static reactors, but the electrode spacing is wide (>1mm), the electrode surface area / reaction liquid volume is relatively small, and it is affected by the Lambert-Beer law, the light penetration is poor, the reaction efficiency is low, and it is not suitable for continuous production. Summary of the invention

[0003] The present invention proposes a new solution to the problems of static reactors in the prior art. We have designed a continuous flow photoelectric reactor with a short electrode spacing and a large surface area / reaction liquid volume ratio. This reactor uses electrode materials commonly used in electrochemistry instead of photosensitive electrodes, and the reaction liquid can continue to pass through the reactor, thereby achieving continuous production. This will help improve the efficiency of molecular photoelectrocatalytic reactions and provide the possibility of continuous production.

[0004] The technical solution adopted by the present invention to solve the technical problem is: construct a continuous flow photoelectrocatalytic reactor, including a photoelectrocatalytic reaction module and an illumination module.

[0005] The photoelectrocatalytic reaction module is composed of a lower box body, an anode plate, a flow channel sheet, a cathode plate, optical glass and an upper cover.

[0006] A flow channel joint is provided on one side of the lower box body, which is used for continuously inputting and outputting the reaction fluid;

[0007] The flow channel sheet is arranged on the upper end surface and the lower end surface of the anode plate, and a flow channel consistent with the flow channel sheet is opened inside the anode plate. The upper cover is a hollow structure in the middle, and receives light through the optical glass to form a light path.

[0008] In some embodiments, the anode plate and cathode plate are non-photosensitive electrodes, such as carbon, metal, etc., to prevent the light source generated by the illumination module from being absorbed by the anode plate and cathode plate, so that the light source can act more fully on the fluid to be reacted.

[0009] In some embodiments, the flow channel structure of the flow channel sheet is a continuous multi-segment curve, and the thickness of the flow channel sheet is less than 1 mm, thereby increasing the surface area / reaction liquid volume ratio and improving the reaction efficiency.

[0010] In some embodiments, the side wall of the lower box body is provided with double through holes for passing the detachable power supply mechanism.

[0011] A double threaded hole is provided on one side wall of the lower box body, and the double threaded hole is used for installing a flow channel joint.

[0012] In some embodiments, the power supply mechanism is an elastic probe having positive and negative electrodes, which is used to realize rapid power supply of the photoelectrocatalytic reaction module.

[0013] In some embodiments, a fluid transport module is further included, which is disposed on one side of the photoelectrocatalytic reaction module.

[0014] The output end of the fluid delivery module is connected to the liquid inlet end of the photoelectrocatalytic reaction module through an infusion hose, so as to provide the photoelectrocatalytic reaction module with fluid to be reacted.

[0015] In some embodiments, the illumination module is provided with a light source, a light source cover plate, and a partition plate.

[0016] The light source is movably fixed to the guide rod by hand screws, and the light source is fixed with a radiator and a second fan.

[0017] The light source can adjust different lighting powers, and the light source can move freely along the guide rod to adjust the lighting position. The hand screw is used to fix the position of the light source on the guide rod, and the partition plate and the light source cover are used to isolate an independent space for the light source.

[0018] In some embodiments, a movable window is provided, one end of which is provided with a rebound button for realizing rotary opening and closing, and the movable window is inlaid with a transparent plate for viewing the illumination module from the inside.

[0019] In some embodiments,

[0020] The circuit control module also includes a control mainboard, a power switch fixed to the bottom plate, and a first fan.

[0021] The power switch is connected to a power source, the power source is fixedly connected to the right side of the motor driver, and the motor driver is fixedly connected to the right side of the electrolytic circuit board.

[0022] The control main board is installed at the rear of the human-machine interaction module, and the electrolytic circuit board is connected to the bottom plate through a circuit fixing plate.

[0023] In some embodiments, the continuous flow photoelectrocatalytic reactor is formed by connecting a front panel, a rear panel, a bottom panel, an upper cover plate, a left side panel and a right side panel.

[0024] The bottom plate and the back plate are in an L-shaped structure, and the left side plate and the upper cover plate are in an L-shaped structure.

[0025] In some embodiments, the human-computer interaction module is further included, which includes a touch screen installed on the front panel and is used to display parameters in the photoelectrocatalytic reaction.

[0026] In the flow-type photoelectrocatalytic reactor described in the present invention, the photoelectrocatalytic reaction module is used to perform photocatalytic, electrochemical and photoelectrocatalytic treatments on the fluid to be reacted. On the one hand, the activity of the test reaction system is orders of magnitude higher than that in the same field. The whole system adopts flow catalysis, which transforms the original static photoelectrocatalysis into dynamic and continuous flow photocatalysis, electrochemistry and photoelectrocatalysis, greatly improving the efficiency of the catalytic reaction, and the product of the catalytic reaction can be obtained in real time;

[0027] On the other hand, the instrument can perform efficient electrosynthesis under low-electrolyte or even electrolyte-free conditions and easily achieve reaction amplification, which is a major breakthrough in the field of photoelectrocatalytic reaction devices. The photoelectrocatalytic reaction module combines sampling, electrolysis and illumination into one, and electrode materials and a variety of flow channels can be freely selected. At the same time, the electrolysis output power is large and the electrolysis output accuracy is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The present invention will be further described below with reference to the accompanying drawings and embodiments, in which:

[0029] Figure 1 It is a schematic diagram of the three-dimensional structure of an embodiment of a flow-type photoelectrocatalytic reactor provided by the present invention;

[0030] Figure 2 It is a schematic diagram of the internal structure of an embodiment of a flow-type photoelectrocatalytic reactor provided by the present invention;

[0031] Figure 3 It is an exploded view of an embodiment of a photoelectrocatalytic reaction module provided by the present invention;

[0032] Figure 4 It is a schematic diagram of a composition reaction implemented by a photoelectrocatalytic reaction module provided by the present invention. DETAILED DESCRIPTION

[0033] In order to have a clearer understanding of the technical features, purposes and effects of the present invention, specific embodiments of the present invention are now described in detail with reference to the accompanying drawings.

[0034] like Figure 1-Figure 3As shown, in the first embodiment of the continuous flow photoelectrocatalytic reactor of the present invention, the continuous flow photoelectrocatalytic reactor includes a human-computer interaction module 200, a fluid delivery module 300, a photoelectrocatalytic reaction module 400, an illumination module 500 and a circuit control module.

[0035] Specifically, the continuous flow photoelectrocatalytic reactor is formed as a rectangular parallelepiped with a hollow structure.

[0036] The front panel 101, the rear panel 102, the upper cover 103 and the right side panel 104 are connected together. The rear panel 102 and the bottom plate form an L-shaped structure, and the upper cover 103 and the left cover form an L-shaped structure.

[0037] Furthermore, the photoelectrocatalytic reaction module 400 is disposed on one side of the continuous flow photoelectrocatalytic reactor, and is used to perform electrocatalysis, photocatalysis and photoelectrocatalysis on the fluid introduced therein to obtain the product of the catalytic reaction.

[0038] Specifically, the photoelectrocatalytic reaction module 400 is formed by stacking a lower box body 401, an anode plate 406, a flow channel sheet 405, a cathode plate 404, an optical glass 407 and an upper cover 409;

[0039] A flow channel joint 412 is provided on one side of the lower box body 401, which is used for inputting and outputting the reaction fluid;

[0040] A flow channel sheet 405 is provided on the upper and lower end surfaces of the anode plate 406 , a flow channel consistent with the flow channel sheet 405 is opened inside the anode plate 406 , and the upper cover 409 is a hollow structure in the middle, receiving light through the optical glass 407 to form a light path.

[0041] For example, Figure 4 Shown ， 1mmol diphenyl ether (Compound 1), 2mmol pyrazole (Compound 2), 0.05mmol 10-methyl-9-mesityl acridine perchlorate, 0.2mmol 2,2,6,6-tetramethylpiperidinoxide and 0.1mmol tetraethylammonium tetrafluoroborate were added to a round-bottom flask, and 12mL 1,2-dichloroethane was added under nitrogen. The inlet tube of the peristaltic pump was inserted into the perforated rubber stopper and quickly replaced with the unperforated rubber stopper of the round-bottom flask. The solution was then bubbled with a nitrogen balloon for 15 minutes. After bubbling, the inlet tube of the peristaltic pump was inserted into the bottom of the solution, and the peristaltic pump of the instrument was turned on and the flow rate was set to 0.2mL min -1 , set the instrument current to 65 mA, turn on the 395 nm light source and adjust the power to 20 W. After the instrument has been running stably for 10 min, start receiving the electrolytic effluent, and the yield of compound 3 is 27%.

[0042] Using this technical solution, the photoelectrocatalytic reaction module is used to perform electrocatalytic, photocatalytic and photoelectrocatalytic treatment on the fluid to be reacted. On the one hand, the activity of the test reaction system is orders of magnitude higher than that of the same field. The whole system adopts flow catalysis, which transforms the original static photoelectrocatalysis into dynamic and continuous flow electrocatalysis, photocatalysis and photoelectrocatalysis, greatly improving the efficiency of the catalytic reaction, and the product of the catalytic reaction can be obtained in real time. In addition, the reaction liquid continuously passes through the reactor, and continuous production can be carried out.

[0043] On the other hand, the instrument can perform efficient electrosynthesis under low-electrolyte or even electrolyte-free conditions and easily achieve reaction amplification, which is a major breakthrough in the field of photoelectrocatalytic reaction devices. The photoelectrocatalytic reaction module combines sampling, electrolysis and illumination into one, and electrode materials and a variety of flow channels can be freely selected. At the same time, the electrolysis output power is large and the electrolysis output accuracy is high.

[0044] In some embodiments, Figure 3 As shown, the material of the anode plate 406 and the cathode plate 404 adopts non-photosensitive electrodes, such as carbon, metal, etc., to avoid the light source generated by the illumination module 500 being absorbed by the anode plate 406 and the cathode plate 404 due to the use of semiconductor photosensitive electrodes with light-absorbing properties. The use of non-photosensitive electrodes can make the light source act more fully on the fluid to be reacted, thereby improving the efficiency of the catalytic reaction.

[0045] In some embodiments, Figure 3 As shown, the flow channel structure of the flow channel sheet 405 is a continuous multi-segment curve. The smaller the flow channel, the longer the time the fluid to be reacted flows in the flow channel sheet, the more complete the contact between the electrode and the sample, and the higher the reaction efficiency. The flow channel structure can be S-shaped or other shapes.

[0046] Among them, the thickness of the flow channel sheet is less than 1 mm, thereby increasing the surface area / reaction liquid volume ratio and improving the reaction efficiency.

[0047] In some embodiments, Figure 3 As shown, a double through hole is provided on the side wall of the lower box body 401 for passing the detachable power supply mechanism, a double threaded hole is provided on one side wall of the lower box body 401 for installing the flow channel connector 412, and a screw 410 is used to fix and lock the photoelectrocatalytic reaction module 400 to prevent leakage.

[0048] Furthermore, the power supply mechanism may use an elastic probe, which (not shown) is provided with positive and negative electrodes, and is used to realize rapid power supply of the photoelectrocatalytic reaction module.

[0049] In some embodiments, in order to ensure the continuity of the fluid to be reacted, a fluid delivery module 300 may be provided in the reactor, which is provided on one side of the photoelectrocatalytic reaction module 400.

[0050] The output end of the fluid delivery module 300 is connected to the liquid inlet end of the photoelectrocatalytic reaction module 400 through a liquid infusion hose, so as to provide the photoelectrocatalytic reaction module with fluid to be reacted.

[0051] The fluid delivery module 300 includes a peristaltic pump and an infusion hose installed on the front panel. The peristaltic pump realizes an adjustable flow function through a touch screen to provide a liquid flow with a stable flow rate for the photoelectrocatalytic reaction module 400.

[0052] The wall thickness of the peristaltic pump infusion hose is 0.86mm, the maximum number of channels is 1, and the number of roller axes is 10.

[0053] In some embodiments, Figure 2 As shown, the reactor further includes an illumination module 500, which includes a light source 501, a light source cover plate 507 and a partition plate 506.

[0054] The light source 501 is movably fixed to the guide rod 504 by means of a hand screw 505. The light source 501 is fixed with a heat sink 502 and a second fan 503.

[0055] The light source 501 can adjust different lighting powers. The light source 501 can move freely along the guide rod 504 to adjust the lighting position. The hand screw 505 is used to fix the position of the light source 501 on the guide rod 504. The partition plate 506 and the light source cover plate 507 are used to isolate an independent space for the light source 501.

[0056] In some embodiments, light source 501 is an LED light source.

[0057] In some embodiments, a movable window 600 is provided on one side of the continuous flow photoelectrocatalytic reactor, and a rebound button 601 is provided at one end of the movable window 600 for realizing rotary opening and closing. The movable window 600 is inlaid with a transparent plate 602 for internal viewing of the illumination module 500.

[0058] In some embodiments, Figure 2 As shown, the circuit control module also includes a control mainboard 704, a power switch 701 fixed to the bottom plate, and a first fan 706.

[0059] The power switch 701 is connected to the power supply 702. The right side of the power supply 702 is fixed to the motor driver 703. The right side of the motor driver 703 is fixedly connected to the electrolytic circuit board 705.

[0060] The control main board 704 is installed at the rear of the human-machine interaction module 200 , and the electrolytic circuit board 705 is connected to the bottom plate via the circuit fixing board 707 .

[0061] In some embodiments, a human-computer interaction module 200 is further included, which includes a touch screen installed on the front panel 101 and is used to display parameters in the photoelectrocatalytic reaction.

[0062] In this embodiment, in the photoelectrocatalytic reaction module, specifically, the material of the anode plate 406 is a graphite plate, the material of the cathode plate 8 is a stainless steel plate, the screws are M4 hexagonal screws, and the sealing flow channel material is FEP.

[0063] The working principle of this embodiment is as follows:

[0064] The peristaltic pump (belonging to the fluid delivery module 300) receives the fluid used for the photoelectrocatalytic reaction and delivers it to the first flow channel connector 412 of the photoelectrocatalytic reaction module through an infusion hose. The reaction fluid passes through the flow channel sheet and is electrocatalyzed by the electrodes composed of the graphite plate 406 and the stainless steel plate 404. In addition, the light path formed by the hollow structure of the upper cover 409 transmits the optical glass 407 to photocatalyze the reaction fluid. Therefore, the reaction fluid is in a dynamic reaction of electrocatalysis and photocatalysis at the same time. After the reaction is complete, the reaction product flows out from the second flow channel connector 412 along the flow channel sheet 405, thereby realizing the dynamic and continuous catalytic fluidization of the photoelectrocatalytic reaction.

[0065] The embodiments of the present invention are described above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned specific implementation modes, which are merely illustrative rather than restrictive. Under the guidance of the present invention, ordinary technicians in this field can also make many forms without departing from the scope of protection of the present invention and the claims, all of which are within the protection of the present invention.

Claims

1. A continuous flow photoelectrocatalytic reactor, characterized in that: It comprises a photoelectrocatalytic reaction module (400) and an illumination module (500), The photoelectrocatalytic reaction module (400) is formed by stacking a lower box body (401), an anode plate (406), a flow channel sheet (405), a cathode plate (404), optical glass (407) and an upper cover (409); A flow channel joint (412) is provided on one side of the lower box body (401) for continuously inputting and outputting the reaction fluid; A double through hole is provided on the side wall of the lower box body (401) for passing a detachable power supply mechanism to supply power to the photoelectrocatalytic reaction module (400); The flow channel sheet (405) is disposed on the upper end surface and the lower end surface of the anode plate (406), a flow channel consistent with the flow channel sheet (405) is opened inside the anode plate (406), and the upper cover (409) is a hollow structure in the middle, receiving light through the optical glass (407) to form a light path; The illumination module (500) provides a light source for the photoelectrocatalytic reaction module (400); The materials of the anode plate (406) and the cathode plate (404) are non-photosensitive electrodes, such as carbon and metal, to prevent the light source generated by the illumination module (500) from being absorbed by the anode plate (406) and the cathode plate (404), so that the light source can act more fully on the fluid to be reacted.

2. The continuous flow photoelectrocatalytic reactor according to claim 1, characterized in that: The flow channel structure of the flow channel sheet (405) is a continuous multi-segment curve; The thickness of the flow channel sheet (405) is less than 1 mm, thereby increasing the surface area / reaction liquid volume ratio.

3. The continuous flow photoelectrocatalytic reactor according to claim 1, characterized in that: A double threaded hole is provided on one side wall of the lower box body (401), and the double threaded hole is used for installing a flow channel connector (412).

4. The continuous flow photoelectrocatalytic reactor according to claim 1, characterized in that: The power supply mechanism is an elastic probe, which is provided with positive and negative electrodes and is used to realize rapid power supply of the photoelectric catalytic reaction module.

5. The continuous flow photoelectrocatalytic reactor according to claim 1, characterized in that: It also includes a fluid transport module (300), which is arranged on one side of the photoelectrocatalytic reaction module (400). The output end of the fluid delivery module (300) is connected to the liquid inlet end of the photoelectrocatalytic reaction module (400) through a liquid infusion hose, so as to provide the photoelectrocatalytic reaction module (400) with fluid to be reacted.

6. The continuous flow photoelectrocatalytic reactor according to claim 1, characterized in that: The illumination module (500) comprises a light source (501), a light source cover plate (507) and a partition plate (506). The light source (501) is movably fixed to the guide rod (504) by means of a hand screw, and the light source is fixed with a heat sink (502) and a second fan (503). The light source (501) can adjust different lighting powers, and the light source (501) can move freely along the guide rod (504) to adjust the lighting position. The hand screw is used to fix the position of the light source (501) on the guide rod (504), and the partition plate (506) and the light source cover plate (507) are used to isolate an independent space for the light source (501).

7. The continuous flow photoelectrocatalytic reactor according to claim 6, characterized in that: A movable window (600) is provided, one end of the movable window (600) is provided with a rebound button (601) for realizing rotary opening and closing, and the movable window (600) is inlaid with a transparent plate (602) for viewing the illumination module (500) from the inside.

8. The continuous flow photoelectrocatalytic reactor according to claim 1, characterized in that: The circuit control module also includes a control mainboard (704), a power switch (701) fixed to the bottom plate, and a first fan (706). The power switch (701) is connected to a power source (702), the power source (702) is fixedly connected to the right side of a motor driver (703), and the motor driver (703) is fixedly connected to the right side of an electrolytic circuit board (705). The control main board is installed at the rear of the human-machine interaction module (200), and the electrolytic circuit board (705) is connected to the bottom plate via a circuit fixing plate (707).

9. The continuous flow photoelectrocatalytic reactor according to claim 1, characterized in that: It also includes the human-computer interaction module (200), which includes a touch screen for displaying parameters in the photoelectrocatalytic reaction.

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