High-flux continuous-flow electrochemical microchannel reaction device and use method thereof

Abstract

The invention discloses a high-flux continuous-flow electrochemical microchannel reaction device and a use method thereof, and belongs to the technical field of microchannel reaction devices, the high-flux continuous-flow electrochemical microchannel reaction device comprises a box body, a graphite plate and a stainless steel plate are arranged in the box body in the vertical direction, and a reaction unit is arranged between the graphite plate and the stainless steel plate in parallel; a platinum sheet is arranged between the reaction unit and the stainless steel plate in parallel, a feeding port and a discharging port are formed in the sides, close to the graphite plate, of the graphite plate and the box body in a penetrating mode, a temperature control unit is arranged on the outer surface of the side wall of the box body, and a detection control unit is arranged on the upper surface of the box body. According to the high-flux continuous-flow electrochemical micro-channel reaction device and the use method thereof, the micro-channel reaction tube is adopted, so that the reaction path is greatly increased under the condition of not changing the size of the electrodes, the distance between the two electrodes is reduced, the voltage during the reaction can be detected in real time, and the detection accuracy is improved. The reaction current and the temperature in the box body are adjusted in time.

Description

Technical Field

[0001] The invention relates to the technical field of microchannel reaction devices, and in particular to a high-throughput continuous-flow electrochemical microchannel reaction device and a use method thereof. Background Art

[0002] A microchannel reactor is a three-dimensional structural element that can be used for chemical reactions and is made of a solid matrix using special micromachining technology. Microchannel reactors usually contain small channel sizes and channel diversity, in which fluids flow and in which the required reactions occur. Microchannel reactors have a very large specific surface area in microstructured chemical equipment, and have better heat and mass transfer capabilities than reactors.

[0003] In the prior art, the electrode spacing of the electrochemical reactor is large, the electrolyte is wasted, and during the reaction process, the reaction voltage cannot be monitored in real time, the current required for the reaction cannot be adjusted in real time, and the temperature inside the reactor may change as the reaction proceeds, thereby affecting the progress and accuracy of the reaction. Summary of the invention

[0004] In order to overcome the shortcomings of the prior art, the purpose of the present invention is to provide a high-throughput continuous flow electrochemical microchannel reaction device and a method of using the same. The microchannel reaction tube is used to greatly increase the reaction path without changing the electrode size, reduce the distance between the two electrodes, and can detect the voltage during the reaction in real time, and timely adjust the reaction current and the internal temperature of the box.

[0005] To achieve the above object, the present invention provides the following solutions:

[0006] A high-throughput continuous-flow electrochemical microchannel reaction device comprises a box body, wherein a graphite plate and a stainless steel plate are arranged vertically inside the box body, a reaction unit is arranged parallel to the middle of the graphite plate and the stainless steel plate, a platinum sheet is arranged parallel to the reaction unit and the stainless steel plate, a material inlet and a material outlet are penetrated through the graphite plate and a side of the box body close to the graphite plate, a temperature control unit is arranged on the outer surface of the side wall of the box body, and a detection control unit is arranged on the upper surface of the box body.

[0007] Preferably, the reaction unit comprises a reaction plate and a microchannel reaction tube, a groove is provided on one side of the reaction plate, and the microchannel reaction tube is embedded in the groove of the reaction plate.

[0008] Preferably, the feed inlet is connected to one end of the microchannel reaction tube, and the discharge port is connected to the other end of the microchannel reaction tube. A three-way feed pipe and a discharge pipe are provided on the outer surface of one side of the box body with the feed inlet and the discharge port, and the three-way feed pipe is detachably connected to the feed inlet, and the discharge pipe is detachably connected to the discharge port.

[0009] Preferably, the temperature control unit includes a condenser, a condensation box and a protective shell. The condenser is arranged in the inner interlayer of the side wall of the box body. The condensation box is fixedly connected to the lower surface of the box body. The condenser is connected to the condensation box through a connecting pipe. The connecting pipe is attached to the outer surface of the side wall of the box body. The protective shell is arranged on the surface of the connecting pipe, and the protective shell is used to protect the connecting pipe.

[0010] Preferably, a first opening and a second opening are provided through the upper surface of the box body, and the first opening and the second opening are symmetrically arranged at two ends of the upper surface of the box body, and the first opening and the second opening are used for the electrode copper rod to enter the interior of the box body and contact and communicate with the graphite plate and the stainless steel plate.

[0011] Preferably, the detection control unit includes an induction ring, an induction column and a detection regulator, the induction ring is fixedly arranged on the inner walls of the first opening and the second opening, the induction column is arranged on the upper surface of the box body, the induction column is respectively located on one side of the first opening and the second opening, the induction column is electrically connected to the induction ring, the lower surface of the detection regulator is provided with an opening, and the induction column is connected to the detection regulator by being embedded in the opening on the lower surface of the detection regulator.

[0012] Preferably, a first insulating plate is provided between the graphite plate and one side of the inner wall of the box body, a second insulating plate is provided between the stainless steel plate and the other side of the inner wall of the box body, a clamping unit is provided between the second insulating plate and the inner wall of the box body, the clamping unit comprises a clamping plate and a locking fixing rod, the locking fixing rod is threadedly connected to the side wall of the box body, the locking fixing rod is rotatably connected to the clamping plate, and the clamping plate is used to control the spacing between components inside the box body.

[0013] The present invention also discloses a method for using the high-throughput continuous-flow electrochemical microchannel reaction device, comprising the following steps:

[0014] S1. First, install the first insulating plate, the graphite plate, the reaction plate, the platinum sheet, the stainless steel plate, and the second insulating plate in the box in sequence, and then seal the box;

[0015] S2, connect the three-way feed pipe to the feed inlet, and connect the discharge pipe to the discharge outlet;

[0016] S3, inserting the electrode copper rods into the first opening and the second opening, and connecting the positive and negative electrodes of the power supply to the two electrode copper rods respectively;

[0017] S4, connecting the opening on the lower surface of the voltage detection controller to the corresponding sensing column;

[0018] S5. Turn on the power switch to energize the electrode copper rod. The reaction liquid enters the box through the three-way feed pipe through the water pump, enters the microchannel reaction tube through the feed port, and flows out from the discharge pipe through the discharge port after the reaction. During the reaction, the temperature inside the box is adjusted by the temperature control unit, and the voltage between the graphite plate and the stainless steel plate is monitored in real time by the voltage detection and adjustment unit, and adjusted at any time. When the reaction is completed, all power supplies are disconnected and use is terminated.

[0019] Therefore, the present invention adopts the above-mentioned high-throughput continuous flow electrochemical microchannel reaction device and its use method, which has the following beneficial effects:

[0020] (1) The present invention adopts a microchannel reaction tube, which greatly increases the reaction path without changing the electrode size and reduces the distance between the two electrodes.

[0021] (2) The present invention can detect the voltage during the reaction in real time and adjust the reaction current in time by setting up a detection device unit.

[0022] (3) The present invention can adjust the internal temperature of the box according to demand by setting a temperature control unit to prevent the temperature change during the reaction process from affecting the reaction effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0024] Figure 1 It is a structural schematic diagram of a high-throughput continuous-flow electrochemical microchannel reaction device of the present invention;

[0025] Figure 2 It is a cross-sectional view of a high-throughput continuous-flow electrochemical microchannel reaction device of the present invention;

[0026] Reference numerals

[0027] 1. Box body; 2. Graphite plate; 3. Stainless steel plate; 4. Reaction unit; 41. Reaction plate; 42. Microchannel reaction tube; 5. Platinum sheet; 6. Feed inlet; 7. Discharge outlet; 8. Temperature control unit; 81. Condenser; 82. Condensation box; 83. Protective shell; 9. Detection control unit; 91. Induction ring; 92. Induction column; 93. Detection regulator; 10. Three-way feed pipe; 11. Discharge pipe; 12. Connecting pipe; 13. First opening; 14. Second opening; 15. First insulating plate; 16. Second insulating plate; 17. Pressing unit; 171. Pressing plate; 172. Locking fixing rod; 18. Electrode copper rod. DETAILED DESCRIPTION

[0028] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] In order to make the purpose, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0030] Embodiment 1

[0031] like Figure 1 to Figure 2 As shown, the present invention provides a high-throughput continuous flow electrochemical microchannel reaction device and a method for using the same, comprising a box body 1, a graphite plate 2 and a stainless steel plate 3 are arranged vertically inside the box body 1, a reaction unit 4 is arranged parallel to the graphite plate 2 and the stainless steel plate 3, a platinum sheet 5 is arranged parallel to the reaction unit 4 and the stainless steel plate 3, an inlet 6 and a discharge port 7 are penetrated through the graphite plate 2 and the side of the box body 1 close to the graphite plate 2, a temperature control unit 8 is arranged on the outer surface of the side wall of the box body 1, and a detection control unit 9 is arranged on the upper surface of the box body 1.

[0032] The reaction unit 4 includes a reaction plate 41 and a microchannel reaction tube 42. A groove is provided on one side of the reaction plate 41. The microchannel reaction tube 42 is embedded in the groove of the reaction plate 41. One end of the microchannel reaction tube 42 is connected to the feed port 6, and the other end of the microchannel reaction tube 42 is connected to the discharge port 7. A three-way feed pipe 10 and a discharge pipe 11 are connected to the outer surface of one side of the box body 1 through which the feed port 6 and the discharge port 7 are provided. The three-way feed pipe 10 is detachably connected to the feed port 6, and the discharge pipe 11 is detachably connected to the discharge port 7.

[0033] The temperature control unit 8 includes a condenser 81, a condenser box 82 and a protective shell 83. The condenser 81 is arranged in the inner interlayer of the side wall of the box body 1. The condenser box 82 is fixedly connected to the lower surface of the box body 1. The condenser 81 and the condenser box 82 are connected through a connecting pipe 12. The connecting pipe 12 is attached to the outer surface of the side wall of the box body 1. The protective shell 83 is arranged on the surface of the connecting pipe 12, and the protective shell 83 is used to protect the connecting pipe 12. The temperature control unit 8 is used to adjust the internal temperature of the box body 1. When the device is powered on for reaction, heat will be generated inside the box body 1, which may affect the progress or effect of the reaction. The temperature control unit 8 can be controlled to adjust and stabilize the internal temperature of the box body 1 to reduce the impact of temperature changes on the reaction.

[0034] The upper surface of the box body 1 is penetrated with a first opening 13 and a second opening 14, which are symmetrically arranged at both ends of the upper surface of the box body 1, and are used for the electrode copper rod 18 to enter the box body 1 and contact and communicate with the graphite plate 2 and the stainless steel plate 3, so as to achieve the conduction of the electrical reaction.

[0035] The detection control unit 9 includes an induction ring 91, an induction column 92 and a detection regulator 93. The induction ring 91 is fixedly arranged on the inner wall of the first opening 13 and the second opening 14. The induction column 92 is arranged on the upper surface of the box body 1. The induction column 92 is located on one side of the first opening 13 and the second opening 14 respectively. The induction column 92 is electrically connected to the induction ring 91. When the electrode copper rod 18 is inserted into the first opening 13 and the second opening 14, the induction ring 91 will contact the electrode copper rod 18. Since the induction column 92 is electrically connected to the induction ring 91, the electrode copper rod 18, the induction ring 91 and the induction column 92 will be connected in series. The lower surface of the detection regulator 93 is provided with an opening, and the induction column 92 is connected to the detection regulator 93 by being embedded in the lower surface opening of the detection regulator 93. At this time, the detection regulator 93 is connected in parallel to the internal reaction circuit of the box 1. When the device is powered on, the detection regulator 93 will detect the voltage during the reaction inside the box 1, and can adjust the current during the reaction inside the box 1 by adjusting the resistance value of the voltage detection device, thereby achieving real-time detection of the voltage and current control during the reaction inside the box 1.

[0036] A first insulating plate 15 is provided between the graphite plate 2 and one side of the inner wall of the box 1, a second insulating plate 16 is provided between the stainless steel plate 3 and the other side of the inner wall of the box 1, a pressing unit 17 is provided between the second insulating plate 16 and the inner wall of the box 1, the pressing unit 17 comprises a pressing plate 171 and a locking and fixing rod 172, the locking and fixing rod 172 is threadedly connected to the side wall of the box 1, the locking and fixing rod 172 is rotatably connected to the pressing plate 171, and the pressing plate 171 is used to control the spacing of the components inside the box 1. This makes the contact between the graphite plate 2, the stainless steel plate 3 and the electrode copper rod 18 tighter.

[0037] The method of using the above-mentioned electrochemical microchannel reaction device is as follows:

[0038] S1, first install the first insulating plate 15, the graphite plate 2, the reaction plate 41, the platinum sheet 5, the stainless steel plate 3, and the second insulating plate 16 in the box body 1 in sequence, and then close the box body 1;

[0039] S2, connect the three-way feed pipe 10 to the feed inlet 6, and connect the discharge pipe 11 to the discharge port 7;

[0040] S3, insert the electrode copper rod 18 into the first opening 13 and the second opening 14, and connect the positive and negative electrodes of the power supply to the two electrode copper rods 18 respectively;

[0041] S4, connecting the lower surface opening of the voltage detection controller to the corresponding sensing column 92;

[0042] S5. Turn on the power switch to energize the electrode copper rod 18. The reaction liquid enters the interior of the box 1 through the three-way feed pipe 10 via the water pump, enters the microchannel reaction tube 42 through the feed port 6, and flows out from the discharge pipe 11 through the discharge port 7 after the reaction. During the reaction, the internal temperature of the box 1 can be adjusted by the temperature control unit 8, and the voltage between the graphite plate 2 and the stainless steel plate 3 can be monitored in real time by the voltage detection and adjustment unit, and the current of the reaction can be adjusted at any time. After the reaction is completed, all power supplies are disconnected and the use is terminated.

[0043] Therefore, through the above-mentioned high-throughput continuous flow electrochemical microchannel reaction device and its use method, a microchannel reaction tube is used to greatly increase the reaction path without changing the electrode size, reduce the distance between the two electrodes, and can detect the voltage during the reaction in real time, and adjust the reaction current and the internal temperature of the box in time.

[0044] The principles and implementation methods of the present invention are described in this article using specific examples. The description of the above embodiments is only used to help understand the method and core idea of ​​the present invention. At the same time, for those skilled in the art, according to the idea of ​​the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A high-throughput continuous-flow electrochemical microchannel reaction device, characterized in that: It comprises a box body, wherein a graphite plate and a stainless steel plate are arranged vertically inside the box body, a reaction unit is arranged parallel to the middle of the graphite plate and the stainless steel plate, a platinum sheet is arranged parallel to the reaction unit and the stainless steel plate, an inlet and an outlet are penetrated through the graphite plate and the side of the box body close to the graphite plate, a temperature control unit is arranged on the outer surface of the side wall of the box body, and a detection control unit is arranged on the upper surface of the box body.

2. A high-throughput continuous-flow electrochemical microchannel reaction device according to claim 1, characterized in that: The reaction unit comprises a reaction plate and a microchannel reaction tube. A groove is arranged on one side of the reaction plate, and the microchannel reaction tube is embedded in the groove of the reaction plate.

3. A high-throughput continuous-flow electrochemical microchannel reaction device according to claim 2, characterized in that: The feed port is connected to one end of the microchannel reaction tube, and the discharge port is connected to the other end of the microchannel reaction tube. A three-way feed pipe and a discharge pipe are provided on the outer surface of one side of the feed port and the discharge port outside the box body, and the three-way feed pipe is detachably connected to the feed port, and the discharge pipe is detachably connected to the discharge port.

4. A high-throughput continuous-flow electrochemical microchannel reaction device according to claim 3, characterized in that: The temperature control unit includes a condenser, a condensation box and a protective shell. The condenser is arranged in the inner interlayer of the side wall of the box body. The condensation box is fixedly connected to the lower surface of the box body. The condenser is connected to the condensation box through a connecting pipe. The connecting pipe is attached to the outer surface of the side wall of the box body. The protective shell is arranged on the surface of the connecting pipe, and the protective shell is used to protect the connecting pipe.

5. A high-throughput continuous-flow electrochemical microchannel reaction device according to claim 4, characterized in that: The upper surface of the box body is penetrated by a first opening and a second opening, which are symmetrically arranged at two ends of the upper surface of the box body, and the first opening and the second opening are used for the electrode copper rod to enter the box body and contact and communicate with the graphite plate and the stainless steel plate.

6. A high-throughput continuous-flow electrochemical microchannel reaction device according to claim 5, characterized in that: The detection control unit includes an induction ring, an induction column and a detection regulator. The induction ring is fixedly arranged on the inner walls of the first opening and the second opening. The induction column is arranged on the upper surface of the box body. The induction column is respectively located on one side of the first opening and the second opening. The induction column is electrically connected to the induction ring. An opening is arranged on the lower surface of the detection regulator. The induction column is connected to the detection regulator by being embedded in the opening on the lower surface of the detection regulator.

7. A high-throughput continuous-flow electrochemical microchannel reaction device according to claim 6, characterized in that: A first insulating plate is provided between the graphite plate and one side of the inner wall of the box body, a second insulating plate is provided between the stainless steel plate and the other side of the inner wall of the box body, a clamping unit is provided between the second insulating plate and the inner wall of the box body, the clamping unit comprises a clamping plate and a locking fixing rod, the locking fixing rod is threadedly connected to the side wall of the box body, the locking fixing rod is rotatably connected to the clamping plate, and the clamping plate is used to control the spacing of the components inside the box body.

8. The method for using a high-throughput continuous-flow electrochemical microchannel reaction device according to any one of claims 1 to 7, characterized in that: The following steps are involved: S1. First, install the first insulating plate, the graphite plate, the reaction plate, the platinum sheet, the stainless steel plate, and the second insulating plate in the box in sequence, and then seal the box; S2, connect the three-way feed pipe to the feed inlet, and connect the discharge pipe to the discharge outlet; S3, inserting the electrode copper rods into the first opening and the second opening, and connecting the positive and negative electrodes of the power supply to the two electrode copper rods respectively; S4, connecting the opening on the lower surface of the voltage detection controller to the corresponding sensing column; S5. Turn on the power switch to energize the electrode copper rod. The reaction liquid enters the box through the three-way feed pipe through the water pump, enters the microchannel reaction tube through the feed port, and flows out from the discharge pipe through the discharge port after the reaction. During the reaction, the temperature inside the box is adjusted by the temperature control unit, and the voltage between the graphite plate and the stainless steel plate is monitored in real time by the voltage detection and adjustment unit, and adjusted at any time. When the reaction is completed, all power supplies are disconnected and use is terminated.

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