An electrochemical reaction cell for Raman and mass spectrometry

Abstract

The invention discloses an electrochemical reaction cell for combining Raman and mass spectrometry, and relates to the technical field of electrochemical reaction cells. The cell comprises a cathode module, which comprises a cathode compartment, wherein a Raman observation window is embedded in the top surface of the cathode compartment, and a window sealing cover is closed on the top of the Raman observation window; a first liquid guide port is opened at the bottom of the cathode compartment; an anode module is sealed and docked with the side of the cathode compartment, and a proton interaction membrane is built into the anode module; an exhaust module comprises a gas derivation block, and the gas derivation block is sealed and docked with the bottom surface of the cathode compartment; a sample sealing unit is embedded in the interior of a containing tank, and the sample sealing unit is used for contacting an electrolyte with a sample and derivatizing a reaction gas; the sample sealing unit comprises a hydrophobic membrane; and a flipping unit. The invention can simultaneously realize in-situ analysis and detection of Raman and mass spectrometry, thereby improving the efficiency of research on the reaction mechanism of the sample.

Description

Technical Field

[0001] The invention relates to the technical field of electrochemical reaction cells, in particular to an electrochemical reaction cell combined with Raman and mass spectrometry. Background Art

[0002] In the field of electrochemical mechanism research, real-time monitoring of changes in electrode surface substances and synergistic analysis of gas products are key technical means to reveal reaction pathways. Existing technologies typically use in-situ Raman spectroscopy to characterize the molecular structure of intermediates adsorbed on the electrode surface, while simultaneously combining mass spectrometry to perform qualitative and quantitative analysis of gas products produced during the reaction. However, conventional electrochemical reaction cells face the following technical challenges in achieving this multimodal detection:

[0003] Most existing devices use a single detection mode design. Most of them are Raman detection-specific electrolytic cells with only optical observation windows, which cannot be simultaneously connected to the mass spectrometry analysis system. If gas analysis is required, a separate mass spectrometry analysis experiment is required. This discrete design makes it impossible for researchers to obtain dynamic correlation data between surface reaction information and gas-phase products in the same reaction process, which restricts the integrity of the mechanism research of complex electrochemical systems. Summary of the Invention

[0004] The object of the present invention is to provide an electrochemical reaction cell for combining Raman and mass spectrometry to solve the problems raised in the prior art.

[0005] To achieve the above-mentioned object, the present invention provides the following technical solution: an electrochemical reaction cell for Raman and mass spectrometry, comprising: a cathode module, which includes a cathode chamber, a Raman observation window embedded in the top surface of the cathode chamber, and a window sealing cover covering the top of the Raman observation window; a first liquid guide port is opened at the bottom of the cathode chamber;

[0006] The anode module is sealed and docked with the side of the cathode chamber, and the anode module has a built-in proton interaction membrane;

[0007] The exhaust module includes a gas outlet block, which is sealed and docked with the bottom surface of the cathode chamber. A receiving groove is provided in the middle of the gas outlet block and is relatively located directly below the first liquid guide port. A negative pressure exhaust connector is provided on the side wall of the gas outlet block. The inner wall of the receiving groove is connected to the negative pressure exhaust connector through a horizontal hole. A sample sealing unit is embedded in the interior of the receiving groove. The sample sealing unit is used to contact the electrolyte with the sample and discharge the reaction gas. The sample sealing unit includes a hydrophobic membrane.

[0008] A turning unit, which is detachably connected to the exhaust module and is used to drive the exhaust module to turn over, so that the exhaust module or the anode module is alternately upright;

[0009] The consumables production unit has a driving end connected to the flipping unit and is used to produce the required proton interactive membrane or hydrophobic membrane during the flipping process.

[0010] Furthermore, the four sides of the cathode chamber are respectively provided with a first liquid inlet joint, a first liquid discharge joint, a reference electrode and a second liquid guide port.

[0011] Furthermore, the anode module includes an anode bin, a counter electrode is installed at one end of the anode bin, a second liquid inlet joint is installed at the other end, a second liquid discharge joint is installed on the top surface of the anode bin, a third liquid guide port is provided on the inner wall of the anode bin, a first sealing gasket, a proton interaction membrane and a second sealing gasket are provided between the anode bin and the cathode bin, the first sealing gasket and the second sealing gasket have the same structure, a fourth liquid guide port is provided in the middle of the first sealing gasket, the proton interaction membrane is placed in the middle between the first sealing gasket and the second sealing gasket, and the proton interaction membrane is used to allow protons in the liquid to flow between the cathode chamber and the anode chamber.

[0012] Furthermore, first through holes are provided at the four corners of the anode bin, a group of first guide rods are passed through each group of first through holes, second through holes are provided at the four corners of the first sealing gasket, the first sealing gasket and the second sealing gasket are both mounted on the first guide rods, the inner ends of the four groups of first guide rods are vertically fixed to the side walls of the cathode bin, the outer ends of the four groups of first guide rods are fixedly connected to the baffle, the outward-moving anode bin is stopped on the inner side of the baffle, and an interference screw is screwed on the center of the baffle.

[0013] Furthermore, the gas derivation block is provided with third through-holes at the four corners, and a group of second guide rods is passed through the interior of each group of third through-holes. The top ends of the four groups of second guide rods are vertically fixedly connected to the cathode bin, and the bottom ends are vertically fixedly connected to the base. The outside of the second guide rods is sheathed with springs, which are placed at the bottom of the gas derivation block. The first and second pressure wheel frames are symmetrically rotatably installed on both sides of the gas derivation block. A base is provided on the bottom surface of the base, and slots are symmetrically provided inside the base, and a flip unit is inserted on the side of the slots.

[0014] When the reaction cell is assembled, the gas outlet block is attached to the bottom of the cathode bin, the anode bin is attached to the side of the cathode bin, the first pressure wheel frame is buckled to the top surface of the cathode bin away from the side of the anode bin, and the second pressure wheel frame is buckled to the outer side of the anode bin. The spring is stretched to quickly complete the positioning of the gas outlet block and the anode bin.

[0015] Furthermore, the sample sealing unit includes a third sealing pad, a fourth sealing pad, a hydrophobic membrane and a porous ceramic sheet arranged from top to bottom. The third sealing pad and the fourth sealing pad adopt the same structure, and the sample is placed between the third sealing pad and the fourth sealing pad; a fifth liquid guide port is opened inside the third sealing pad.

[0016] Furthermore, the flip unit includes a support plate, two groups of first side plates are vertically provided on the surface of the support plate, an active roller is provided on the top between the two groups of first side plates, an assembly frame is symmetrically fixed to the outer wall of the active roller, and the assembly frame includes an inclined rod and an insertion rod, one end of the inclined rod is fixedly connected to the active roller, and the other end of the inclined rod is connected to the constraint plate, the side wall of the constraint plate is connected to the insertion rod, the insertion rod is horizontally inserted into the slot and the end is positioned by a nut; the active roller drives the assembly frame to rotate so that the gas outlet block or the anode bin is vertical; two groups of second side plates are vertically provided on the surface of the support plate, the second side plates are located on the outside of the first side plates, and a storage plate is provided on the top of the two groups of second side plates.

[0017] Furthermore, the consumables production unit includes a first storage wheel, a second storage wheel, a first cutting component, a second cutting component and a side driving component. The first storage wheel and the second storage wheel are installed between the two groups of second side plates. The first storage wheel is located above the second storage wheel. The outer wall of the first storage wheel is wrapped with a proton interactive coil, and the outer wall of the second storage wheel is wrapped with a hydrophobic coil; the output end of the proton interactive coil is provided with a first cutting component, and the output end of the hydrophobic coil is provided with a second cutting component, and the input end of the side driving component is connected to the active roller; when the active roller drives the exhaust module to load vertically, the side driving component drives the second cutting component to cut out the hydrophobic film; when the active roller drives the anode module to load vertically, the side driving component drives the first cutting component to cut out the proton interactive membrane.

[0018] Furthermore, the side driving component includes a driven roller, a movable tooth plate and a side fixed plate. The driven roller is arranged between the two groups of first side plates and is located at the bottom of the active roller. The two ends of the active roller are connected to the driven roller through a first transmission belt. The driven roller is connected to the driven wheel through a second transmission belt. The side wall of the driven wheel is provided with a driving gear. The movable tooth plate is vertically slid and placed on the side wall of the side fixed plate. The driving gear is meshed and connected with the movable tooth plate. The side fixed plate is symmetrically placed on the support plate.

[0019] Furthermore, the first cutting component includes a first cutting frame and a first constraint frame, the output end of the proton interactive coil passes through the first constraint frame, the top surface of the first constraint frame is provided with a first incision, the first cutting frame is located directly above the first incision, the two sides of the first cutting frame are connected to the top of the inner wall of the movable tooth plate, and the two ends of the first constraint frame are connected to the top of the inner wall of the side fixed plate; the second cutting component includes a second cutting frame and a second constraint frame, the output end of the hydrophobic coil passes through the second constraint frame, the bottom surface of the second constraint frame is provided with a second incision, a second cutting frame is provided directly below the second incision, the two ends of the second cutting frame are connected to the bottom of the inner wall of the movable tooth plate, and the two ends of the second constraint frame are connected to the bottom of the inner wall of the side fixed plate; both ends of the first cutting frame and the second cutting frame are open structures.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] 1. The above-mentioned electrochemical reaction cell can simultaneously realize in-situ analysis and detection of Raman (surface substances) and mass spectrometry (gas products), improving the efficiency of research on sample reaction mechanisms, eliminating the need to use two sets of equipment to complete analysis and detection separately; electrochemical reactions such as hydrogen evolution and CO2 reduction;

[0022] 2. The overall three-dimensional design of each module is convenient for the placement of internal materials of the module and for subsequent docking, which can simplify the connection of liquid and gas lines and facilitate maintenance;

[0023] 3. The gas derivation module is equipped with a sample sealing unit to encapsulate the sample, which can ensure that there is no leakage of the electrolyte and at the same time ensure the directional transmission of the gas. A negative pressure drain joint is provided on the outside of the gas derivation block, which can extract the reaction gas under negative pressure, thereby improving the gas collection speed and mass spectrometry sensitivity. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 Schematic diagram of the structure of the electrochemical reaction cell for Raman and mass spectrometry coupling of the present invention;

[0025] Figure 2 This is a schematic diagram of the overall explosion structure of the electrochemical reaction cell of the present invention;

[0026] Figure 3 Schematic diagram of the cathode chamber structure of the present invention;

[0027] Figure 4 Schematic diagram of the anode module structure of the present invention;

[0028] Figure 5 This is a schematic diagram of the docking structure of the electrochemical reaction cell and the flip unit of the present invention;

[0029] Figure 6 This is a schematic diagram of the vertical state structure of the anode chamber of the present invention;

[0030] Figure 7 This is a schematic structural diagram of the electrochemical reaction cell in the docking state of the present invention;

[0031] Figure 8 This is a schematic diagram of the structure of the flip unit of the present invention;

[0032] Figure 9 This is a schematic diagram of the active roller connection structure of the present invention;

[0033] Figure 10 This is a schematic diagram of the side cross-sectional structure of the consumables manufacturing unit of the present invention;

[0034] Figure 11 Schematic diagram of the structure of the first cutting component and the second cutting component of the present invention;

[0035] Figure 12 This is a schematic diagram of a top cross-sectional structure of a consumables manufacturing unit of the present invention;

[0036] Figure 13 This is a schematic structural diagram of the first storage roller and the second storage roller of the present invention.

[0037] Reference numerals:

[0038] 100, cathode module, 110, cathode chamber, 111, first liquid guide port, 112, second liquid guide port, 120, Raman observation window, 130, window sealing cover, 140, reference electrode, 150, first liquid inlet connector, 160, first liquid outlet connector,

[0039] 200, anode module, 210, anode chamber, 211, third liquid guide port, 212, first through hole, 220, second liquid inlet connector, 230, second liquid outlet connector, 240, counter electrode, 250, first sealing gasket, 251, second through hole, 252, fourth liquid guide port, 260, second sealing gasket, 270, proton interaction membrane, 280, first guide rod, 290, baffle, 291, contact screw,

[0040] 300, exhaust module, 310, gas outlet block, 311, receiving tank, 312, negative pressure exhaust connector, 320, sample sealing unit, 321, third sealing gasket, 322, fourth sealing gasket, 323, hydrophobic membrane, 324, porous ceramic sheet, 325, fifth liquid guide port,

[0041] 330, second guide rod, 331, spring, 340, base, 350, base, 351, slot, 360, first pressure wheel frame, 370, second pressure wheel frame,

[0042] 400, turning unit, 410, supporting plate, 420, first side plate, 430, driving roller, 440, assembly frame, 441, inclined rod, 442, restraining plate, 443, inserting rod, 444, nut, 450, second side plate, 460, storage plate,

[0043] 500, consumable material production unit, 510, first storage wheel, 520, second storage wheel,

[0044] 530, first cutting component, 531, first cutting frame, 532, first constraint frame, 533, first incision,

[0045] 540, second cutting component, 541, second cutting frame, 542, second constraint frame, 543, second incision,

[0046] 550, side driving component, 551, driven roller, 552, first transmission belt, 553, second transmission belt, 554, driven wheel, 555, driving gear, 556, movable gear plate, 557, side fixed plate,

[0047] 600, proton interactive coil, 700, hydrophobic coil, 800, sample. DETAILED DESCRIPTION

[0048] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. 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 making creative efforts are within the scope of protection of the present invention.

[0049] Embodiment: The present invention provides a technical solution of an electrochemical reaction cell combined with Raman and mass spectrometry, such as Figures 1-13 As shown, it includes: a cathode module 100, which includes a cathode chamber 110, a Raman observation window 120 embedded in the top surface of the cathode chamber 110, and a window sealing cover 130 covering the top of the Raman observation window 120; a first liquid guide port 111 is opened at the bottom of the cathode chamber 110; and a reference electrode 140 is built into the cathode chamber 110;

[0050] The anode module 200 is sealed and docked with the side of the cathode chamber 110 and has a built-in counter electrode 240;

[0051] The exhaust module 300 includes a gas outlet block 310, which is sealed and docked with the bottom surface of the cathode chamber 110. A receiving groove 311 is defined in the middle of the gas outlet block 310 and is positioned directly below the first liquid guide port 111. A negative pressure exhaust connector 312 is provided on the sidewall of the gas outlet block 310. The inner wall of the receiving groove 311 is connected to the negative pressure exhaust connector 312 via a horizontal hole. A sample sealing unit 320 is embedded in the receiving groove 311. The sample sealing unit 320 is used to allow the electrolyte to contact the sample and extract the reaction gas.

[0052] The turning unit 400 is detachably connected to the exhaust module 300 and is used to drive the exhaust module 300 to turn over, so that the exhaust module 300 or the anode module 200 is alternately vertical;

[0053] The consumables making unit 500 is placed in the flipping unit 400 to make test consumables during the flipping process. The negative pressure exhaust connector is connected to the mass spectrometer through an air pipe.

[0054] In the above scheme:

[0055] 1. The above-mentioned electrochemical reaction cell can simultaneously realize in-situ analysis and detection of Raman (surface substances) and mass spectrometry (gas products), improving the efficiency of research on sample reaction mechanisms, eliminating the need to use two sets of equipment to complete analysis and detection separately; electrochemical reactions such as hydrogen evolution and CO2 reduction;

[0056] 2. The overall three-dimensional design of each module is convenient for the placement of internal materials of the module and for subsequent docking, which can simplify the connection of liquid and gas lines and facilitate maintenance;

[0057] 3. The gas derivation module is equipped with a sample sealing unit 320 to encapsulate the sample, which can ensure that there is no leakage of the electrolyte and at the same time ensure the directional transmission of the gas. The outer side of the gas derivation block 310 is provided with a negative pressure drainage joint, which can extract the reaction gas under negative pressure, thereby improving the gas collection speed and mass spectrometry sensitivity.

[0058] 4. The anode module 200 is side-mounted, making it difficult to place the various accessories. To address this issue, a flip unit 400 is provided. The flip unit 400 can drive the exhaust module 300 to rotate, so that the exhaust module 300 or the anode module 200 is alternately vertical. In this way, when the exhaust module 300 is vertical, the tester can place the exhaust accessories one by one from bottom to top. Similarly, when the anode module 200 is vertical, the tester can also place the anode accessories from bottom to top.

[0059] 5. The consumables production unit 500 can produce the proton interaction membrane and hydrophobic membrane 323 required for each test, without the need for manual cutting and production. When the flipping unit 400 flips, it can drive the consumables production unit 500 to move, so that the consumables production unit 500 can automatically complete the cutting action without waiting. After the flipping is completed, the experimenter can directly remove the cut film.

[0060] As a preferred embodiment, the four sides of the cathode chamber 110 are respectively provided with a first liquid inlet connector 150, a first liquid outlet connector 160, a reference electrode 140, and a second liquid inlet 112. During the test, the electrolyte is input into the cathode chamber 110 through the first liquid inlet connector 150 and then output through the first liquid outlet connector 160. The electrolyte can be transferred to the holding tank 311 through the first liquid outlet 111. The Raman spectrometer monitors the changes in the surface material of the reference electrode 140 in real time through the quartz window.

[0061] As a preferred embodiment, the anode module 200 includes an anode chamber 210, a counter electrode 240 is installed at one end of the anode chamber 210, a second liquid inlet joint 220 is installed at the other end, a second liquid discharge joint 230 is installed on the top surface of the anode chamber 210, and a third liquid guide port 211 is provided on the inner wall of the anode chamber 210. A first sealing gasket 250, a proton interaction membrane 270 and a second sealing gasket 260 are provided between the anode chamber 210 and the cathode chamber 110. The first sealing gasket 250 and the second sealing gasket 260 have the same structure. A fourth liquid guide port 252 is provided in the middle of the first sealing gasket 250, and the proton interaction membrane 270 is placed in the middle between the first sealing gasket 250 and the second sealing gasket 260. The proton interaction membrane 270 is used to allow protons in the liquid to flow between the cathode chamber and the anode chamber. The electrolyte enters the anode compartment 210 through the second liquid inlet connector 220 and is then output through the second liquid discharge connector 230. The protons in the cathode compartment 110 and the anode compartment 210 circulate through the proton interaction membrane 270. The first sealing gasket 250 and the second sealing gasket 260 can achieve a double-layer seal to prevent liquid leakage. The area of ​​the proton interaction membrane 270 is larger than the cross-section of the fourth liquid guide port.

[0062] As a preferred embodiment, the anode bin 210 is provided with first through-holes 212 at the four corners, each set of first through-holes 212 having a set of first guide rods 280 passing through it, and the first sealing gasket 250 is provided with second through-holes 251 at the four corners. The first sealing gasket 250 and the second sealing gasket 260 are both mounted on the first guide rods 280. The inner ends of the four sets of first guide rods 280 are vertically fixed to the side walls of the cathode bin 110, and the outer ends of the four sets of first guide rods 280 are fixedly connected to the baffle 290. The outward-moving anode bin 210 is stopped on the inner side of the baffle 290, and an interference screw 291 is screwed onto the center of the baffle 290. The first sealing gasket 250, the second sealing gasket 260, and the anode bin 210 are all mounted on the first guide rods 280, realizing the storage of the three components. There is no need to store them separately elsewhere. The experimenter only needs to place the proton interaction membrane 270.

[0063] The first guide rod 280 can prevent the first sealing gasket 250, the second sealing gasket 260 and the anode bin 210 from falling when flipping;

[0064] After the anode chamber 210 is rotated to vertical, the experimenter can easily place the proton interaction membrane 270 between the first sealing gasket 250 and the second sealing gasket 260, and then rotate the contact screw 291 to push the anode chamber 210 upward, so that the first sealing gasket 250, the proton interaction membrane 270, the second sealing gasket 260 and the anode chamber 210 are tightly fitted to the side wall of the cathode chamber 110, so as to avoid the proton interaction membrane 270 from being offset when it is subsequently flipped upward.

[0065] As a preferred embodiment, the sample sealing unit 320 includes a third sealing gasket 321, a fourth sealing gasket 322, a hydrophobic membrane 323, and a porous ceramic sheet 324, arranged sequentially from top to bottom. The third sealing gasket 321 and the fourth sealing gasket 322 have the same structure, and the sample 800 is placed between the third sealing gasket 321 and the fourth sealing gasket 322. A fifth liquid guide port 325 is defined within the third sealing gasket 321. The third sealing gasket 321 and the fourth sealing gasket 322 seal and position the sample so that the electrolyte can only contact the sample through the fifth liquid guide port 325. The gas generated by the reaction can be discharged through the hydrophobic membrane 323, while the liquid is blocked by the hydrophobic membrane 323.

[0066] As a preferred embodiment, the proton interaction membrane is Nafion 117; the hydrophobic breathable membrane is made of PTFE; the porous ceramic has a pore size of 10-50 μm; and each sealing gasket is made of silicone.

[0067] The traditional module docking is positioned by bolt assembly, which is cumbersome to operate. The following solution is provided for quickly positioning the anode bin 210 and the gas outlet module: the gas outlet block 310 is provided with third through-holes at the four corners, and each set of third through-holes is penetrated by a set of second guide rods 330. The top ends of the four sets of second guide rods 330 are vertically fixedly connected to the cathode bin 110, and the bottom ends are vertically fixedly connected to the base 340. The outside of the second guide rods 330 is sheathed with springs 331, which are placed at the bottom of the gas outlet block 310. The first pressure wheel frames 360 are symmetrically mounted on both sides of the gas outlet block 310 for rotation. and a second pressure roller frame 370; a base 350 is provided on the bottom surface of the base 340, and a slot 351 is symmetrically provided inside the base 350, and a flip unit 400 is inserted on the side of the slot 351; when the reaction cell is assembled, the gas lead-out block 310 is attached to the bottom surface of the cathode bin 110, and the anode bin 210 is attached to the side of the cathode bin 110, the first pressure roller frame 360 ​​is buckled on the side of the top surface of the cathode bin 110 away from the anode bin 210, and the second pressure roller frame 370 is buckled on the outer side of the anode bin 210, and the spring 331 is stretched to quickly complete the positioning of the gas lead-out block 310 and the anode bin 210.

[0068] 1. The second guide rod 330 can support and position the cathode bin 110. In this way, the position of the cathode bin 110 can be determined by simply docking the gas outlet block 310 and the anode bin 210 on the side wall of the cathode bin 110.

[0069] 2. When the gas derivation block 310 is docked with the bottom surface of the cathode bin 110, the spring 331 can be stretched, and the test personnel buckle the first pressure roller frame 360 ​​and the second pressure roller frame 370. The spring 331 and the pressure roller frame constrain the gas derivation block 310 up and down to achieve rapid positioning of the gas derivation block 310. At the same time, the second pressure roller frame 370 presses on the side of the anode bin 210 to achieve secondary positioning of the anode bin 210.

[0070] In order to realize the flipping of the base 350 and the switching of the loading, the following scheme is given: the flip unit 400 includes a supporting plate 410, the surface of the supporting plate 410 is vertically provided with two groups of first side plates 420, the top of the two groups of first side plates 420 is provided with an active roller 430, the outer wall of the active roller 430 is symmetrically fixed with an assembly frame 440, the assembly frame 440 includes an inclined rod 441 and an insertion rod 443, one end of the inclined rod 441 is fixedly connected to the active roller 430, and the other end of the inclined rod 441 is fixedly connected to the active roller 430. One end is connected to the constraint plate 442, and the side wall of the constraint plate 442 is connected to the insertion rod 443. The insertion rod 443 is horizontally inserted into the slot 351 and the end is positioned by the nut 444; the active roller 430 drives the assembly frame 440 to rotate so that the gas outlet block 310 or the anode bin 210 is vertical; two groups of second side plates 450 are vertically provided on the surface of the support plate 410, and the second side plates 450 are located on the outside of the first side plate 420, and the top of the two groups of second side plates 450 is provided with a storage plate 460.

[0071] 1. The test tools, the third sealing gasket 321, the fourth sealing gasket 322, the porous ceramic sheet 324, etc. can be placed on the storage plate 460;

[0072] 2. The base 350 and the reaction cell above it can be disassembled for maintenance or work independently, and can also be docked with the insertion rod 443. When docking, the insertion rod 443 is inserted into the slot 351, the restraining plate 442 stops the base 350, and then the nut 444 is screwed onto the end of the insertion rod 443 to achieve the clamping and positioning of the base 350;

[0073] 3. The rotation of the active roller 430 can drive the insertion rod 443 to rotate through the inclined rod 441, and the insertion rod 443 drives the base 350 to flip, thereby driving the gas outlet block 310 and the anode compartment 210 to rotate and switch.

[0074] In order to achieve rapid preparation of consumables, the following solution is provided: the consumables production unit 500 includes a first storage wheel 510, a second storage wheel 520, a first slitting component 530, a second slitting component 540 and a side driving component 550. The first storage wheel 510 and the second storage wheel 520 are installed between the two sets of second side plates 450. The first storage wheel 510 is located above the second storage wheel 520. The outer wall of the first storage wheel 510 is wrapped with a proton interactive coil 600, and the outer wall of the second storage wheel 520 is wrapped with a hydrophobic The output end of the proton interaction coil 600 is provided with a first slitting component 530, and the output end of the hydrophobic coil 700 is provided with a second slitting component 540. The input end of the side drive component 550 is connected to the active roller 430. When the active roller 430 drives the exhaust module 300 to load the material vertically, the side drive component 550 drives the second slitting component 540 to cut out the hydrophobic membrane 323. When the active roller 430 drives the anode module 200 to load the material vertically, the side drive component 550 drives the first slitting component 530 to cut out the proton interaction membrane 270. The side drive component 550 can transmit the rotational force of the active roller 430 to the first slitting component 530 and the second slitting component 540, thereby realizing the automatic cutting operation of the first slitting component 530 and the second slitting component 540.

[0075] As a preferred embodiment, the side driving component 550 includes a driven roller 551, a movable tooth plate 556 and a side fixed plate 557. The driven roller 551 is arranged between the two groups of first side plates 420 and is located at the bottom of the active roller 430. The two ends of the active roller 430 are connected to the driven roller 551 through a first transmission belt 552. The driven roller 551 is connected to the driven wheel 554 through a second transmission belt. The side wall of the driven wheel 554 is provided with a driving gear 555. The movable tooth plate 556 is vertically slidably placed on the side wall of the side fixed plate 557. The driving gear 555 is meshed and connected with the movable tooth plate 556. The side fixed plate 557 is symmetrically placed on the support plate 410.

[0076] As a preferred embodiment, the first slitting component 530 includes a first cutting frame 531 and a first constraining frame 532. The output end of the proton interactive coil 600 passes through the first constraining frame 532. The top surface of the first constraining frame 532 is provided with a first incision 533. The first cutting frame 531 is located directly above the first incision 533. The two sides of the first cutting frame 531 are connected to the top of the inner wall of the movable tooth plate 556. The two ends of the first constraining frame 532 are connected to the top of the inner wall of the side fixing plate 557. The second slitting component 540 includes a second cutting frame 541 and a second constraint frame 542. The output end of the hydrophobic coil 700 passes through the second constraint frame 542. A second incision 543 is provided on the bottom surface of the second constraint frame 542. A second cutting frame 541 is provided directly below the second incision 543. The two ends of the second cutting frame 541 are connected to the bottom of the inner wall of the movable tooth plate 556, and the two ends of the second constraint frame 542 are connected to the bottom of the inner wall of the side fixed plate 557; both ends of the first cutting frame 531 and the second cutting frame 541 are open structures.

[0077] During specific implementation, the flip unit 400 and the consumable material production unit 500:

[0078] S1. Pull the end of the hydrophobic membrane 323 coil so that the portion to be cut is placed at the second incision 543, and pull the end of the proton interaction coil 600 so that the portion to be cut is placed at the first incision 533;

[0079] S2. Placement of proton interaction membrane 270:

[0080] The active roller 430 drives the assembly frame 440 to rotate clockwise, causing the anode bin 210 to rotate to a vertical state. During the rotation process, the active roller 430 drives the driven roller 551 to rotate via the first transmission belt 552. The driven roller 551 drives the driven wheel 554 to rotate via the second transmission belt 553. The driven wheel 554 drives the driving gear 555 to rotate. The driving gear 555 rotates clockwise, driving the movable tooth plate 556 to move downward along the side fixed plate 557. The movable tooth plate 556 drives the first cutting frame 531 downward into the first incision 533, thereby cutting out the proton interactive membrane 270. The experimenter removes the proton interactive membrane 270 from above the first cutting frame 531.

[0081] The test personnel placed the proton interaction membrane 270 between the first sealing gasket 250 and the second sealing gasket 260, and rotated the abutment screw 291 to lift the anode chamber 210 into position.

[0082] S3. Placement of hydrophobic membrane 323:

[0083] The active roller 430 drives the assembly frame 440 to rotate counterclockwise, causing the gas deflection block 310 to rotate to a vertical position. During the rotation process, the active roller 430 drives the driven roller 551 to rotate via the first transmission belt 552. The driven roller 551 drives the driven wheel 554 to rotate via the second transmission belt 553. The driven wheel 554 drives the driving gear 555 to rotate. The driving gear 555 rotates counterclockwise, driving the movable tooth plate 556 to move upward along the side fixing plate 557. The movable tooth plate 556 drives the second cutting frame 541 upward into the second incision 543, thereby cutting out the hydrophobic film 323. The tester removes the hydrophobic film 323 from under the second cutting frame 541.

[0084] The porous ceramic sheet 324 , the hydrophobic membrane 323 , the fourth sealing gasket 322 , the sample, and the third sealing gasket 321 are sequentially placed in the receiving tank 311 .

[0085] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be included therein. Any reference sign in a claim should not be construed as limiting the claim to which it relates.

Claims

1. A Raman and mass spectrometry electrochemical reaction cell, characterized in that: include: The cathode module comprises a cathode chamber, a Raman observation window is embedded in the top surface of the cathode chamber, and a window sealing cover is covered on the top of the Raman observation window; A first liquid guide port is provided at the bottom of the cathode chamber; The anode module is sealed and docked with the side of the cathode chamber, and the anode module has a built-in proton interaction membrane; The exhaust module includes a gas outlet block, which is sealed and docked with the bottom surface of the cathode chamber. A receiving groove is provided in the middle of the gas outlet block and is relatively located directly below the first liquid guide port. A negative pressure exhaust connector is provided on the side wall of the gas outlet block. The inner wall of the receiving groove is connected to the negative pressure exhaust connector through a horizontal hole. A sample sealing unit is embedded in the interior of the receiving groove. The sample sealing unit is used to contact the electrolyte with the sample and discharge the reaction gas. The sample sealing unit includes a hydrophobic membrane. A turning unit, which is detachably connected to the exhaust module and is used to drive the exhaust module to turn over, so that the exhaust module or the anode module is alternately upright; A consumables production unit, whose driving end is connected to the flipping unit, is used to produce the required proton interactive membrane or hydrophobic membrane during the flipping process; The anode module includes an anode bin, wherein four corners of the anode bin are provided with first through-holes, each set of the first through-holes penetrates a set of first guide rods, a first sealing gasket and a second sealing gasket are both fitted on the first guide rods, the inner ends of the four sets of first guide rods are vertically fixed to the side walls of the cathode bin, and the outer ends of the four sets of first guide rods are fixedly connected to a baffle, and an interference screw is screwed at the center of the baffle; The gas derivation block is provided with third through-holes at the four corners, and a group of second guide rods is passed through the inside of each group of third through-holes. The top ends of the four groups of second guide rods are vertically fixedly connected to the cathode bin, and the bottom ends are vertically fixedly connected to the base. The outside of the second guide rods is sheathed with springs, which are placed at the bottom of the gas derivation block. The first and second pressure wheel frames are symmetrically mounted on both sides of the gas derivation block. A base is provided on the bottom surface of the base, and slots are symmetrically arranged inside the base, and a flip unit is inserted on the side of the slots. The turning unit includes a supporting plate, on the surface of which two groups of first side plates are vertically provided, and an active roller is provided on the top between the two groups of first side plates; the consumable material production unit includes a first storage wheel, a second storage wheel, a first slitting component, a second slitting component and a side driving component, the first storage wheel and the second storage wheel are installed between the two groups of second side plates, the first storage wheel is located above the second storage wheel, the outer wall of the first storage wheel is wound with a proton interactive coil, and the outer wall of the second storage wheel is wound with a hydrophobic coil; the output end of the proton interactive coil is provided with a first slitting component, the output end of the hydrophobic coil is provided with a second slitting component, and the input end of the side driving component is connected to the active roller; when the active roller drives the exhaust module to vertically load the material, the side driving component drives the second slitting component to cut out the hydrophobic film; When the active roller drives the anode module to be loaded vertically, the side driving component drives the first cutting component to cut out the proton interaction membrane.

2. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 1, characterized in that: The four sides of the cathode chamber are respectively provided with a first liquid inlet joint, a first liquid discharge joint, a reference electrode and a second liquid guide port.

3. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 2, characterized in that: A counter electrode is installed at one end of the anode chamber and a second liquid inlet joint is installed at the other end. A second liquid discharge joint is installed on the top surface of the anode chamber. A third liquid guide port is provided on the inner wall of the anode chamber. A first sealing gasket, a proton interaction membrane and a second sealing gasket are provided between the anode chamber and the cathode chamber. The first sealing gasket and the second sealing gasket have the same structure. A fourth liquid guide port is provided in the middle of the first sealing gasket. The proton interaction membrane is placed in the middle between the first sealing gasket and the second sealing gasket. The proton interaction membrane is used to allow protons in the liquid to flow between the cathode chamber and the anode chamber.

4. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 3, characterized in that: Second through holes are provided at the four corners of the first sealing gasket, and the outward-moving anode bin is stopped on the inner side of the baffle.

5. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 4, characterized in that: When the reaction cell is assembled, the gas outlet block is attached to the bottom of the cathode bin, the anode bin is attached to the side of the cathode bin, the first pressure wheel frame is buckled to the top surface of the cathode bin away from the side of the anode bin, and the second pressure wheel frame is buckled to the outer side of the anode bin. The spring is stretched to quickly complete the positioning of the gas outlet block and the anode bin.

6. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 1, characterized in that: The sample sealing unit includes a third sealing pad, a fourth sealing pad, a hydrophobic membrane and a porous ceramic sheet arranged in sequence from top to bottom. The third sealing pad and the fourth sealing pad adopt the same structure, and the sample is placed between the third sealing pad and the fourth sealing pad; a fifth liquid guide port is opened inside the third sealing pad.

7. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 1, characterized in that: An assembly frame is symmetrically fixed to the outer wall of the active roller, and the assembly frame includes an inclined rod and an insertion rod. One end of the inclined rod is fixedly connected to the active roller, and the other end of the inclined rod is connected to the constraint plate. The side wall of the constraint plate is connected to the insertion rod, and the insertion rod is horizontally inserted into the slot and the end is positioned by a nut; the active roller drives the assembly frame to rotate so that the gas outlet block or the anode bin is vertical; two groups of second side plates are vertically provided on the surface of the support plate, the second side plates are located on the outside of the first side plates, and the top of the two groups of second side plates are provided with a storage plate.

8. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 7, characterized in that: The side driving component includes a driven roller, a movable tooth plate and a side fixed plate. The driven roller is arranged between the two groups of first side plates and is located at the bottom of the active roller. The two ends of the active roller are connected to the driven roller through a first transmission belt. The driven roller is connected to the driven wheel through a second transmission belt. The side wall of the driven wheel is provided with a driving gear. The movable tooth plate is vertically slid and placed on the side wall of the side fixed plate. The driving gear is meshed and connected with the movable tooth plate. The side fixed plate is symmetrically placed on the support plate.

9. The electrochemical reaction cell for Raman spectroscopy combined with mass spectrometry according to claim 8, characterized in that: The first cutting component includes a first cutting frame and a first constraint frame. The output end of the proton interactive coil passes through the first constraint frame. A first incision is opened on the top surface of the first constraint frame. The first cutting frame is located directly above the first incision. Both sides of the first cutting frame are connected to the top of the inner wall of the movable tooth plate, and the two ends of the first constraint frame are connected to the top of the inner wall of the side fixed plate; the second cutting component includes a second cutting frame and a second constraint frame. The output end of the hydrophobic coil passes through the second constraint frame. A second incision is opened on the bottom surface of the second constraint frame. A second cutting frame is provided directly below the second incision. Both ends of the second cutting frame are connected to the bottom of the inner wall of the movable tooth plate, and the two ends of the second constraint frame are connected to the bottom of the inner wall of the side fixed plate; both ends of the first cutting frame and the second cutting frame are open structures.

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