Constant-temperature electrochemical constant-voltage electrolysis device and test method

Abstract

The invention discloses a constant-temperature electrochemical constant-voltage electrolysis device and a testing method, and belongs to the technical field of electrochemical testing and electrosynthesis. The electrolysis device comprises an electrolytic tank main body, an electrode system, a sealing system and an electrochemical workstation, when the electrolysis device is used for electrochemical testing and synthesis, a constant temperature system and a sealing ventilation structure are integrated, inert / reactive gas is introduced in a compatible mode, and accurate potential control and electrolytic reaction are carried out under the constant temperature condition; according to the device, the module integration design is adopted, the distance and the space layout of the working electrode and the counter electrode are fixed, the electric field distribution consistency is ensured, the experiment repeatability and the data reliability are effectively improved, and meanwhile the experiment operation process is further simplified.

Description

Technical Field

[0001] This invention belongs to the field of electrochemical testing and electrosynthesis technology, specifically relating to a constant-temperature and constant-voltage electrolysis device and testing method for electrochemical research and synthesis. The device integrates precise temperature control, inert atmosphere management, a multi-electrode system, and in-situ testing functions. It features a compact structure, simple operation, and is suitable for various applications ranging from electrochemical analysis to controlled-potential synthesis. Background Technology

[0002] In the field of electrosynthesis research, such as the electrochemical conversion of organic molecules and the organic electrosynthesis of fine chemicals, three-electrode electrolytic cells are indispensable core devices for achieving precise potential control. Currently, traditional electrolytic cells commonly used in laboratories typically rely on on-site temporary assembly of components such as flasks, independent electrode ports, and gas supply pipes. However, this non-standardized assembly mode has the following inherent defects, severely restricting the accuracy and reproducibility of research data and increasing the complexity of experimental operations: inconsistent electrode spacing and spatial layout lead to poor experimental repeatability; lack of integrated temperature control systems affects data accuracy; poor gas environment control and sealing performance limit the research scope and pose a risk of contamination; and single-chamber design easily leads to cross-interference of reaction products between electrodes. In summary, the inherent deficiencies of traditional temporary assembled electrolytic cells in terms of accuracy, repeatability, safety, and functionality have become a bottleneck restricting the efficiency and data quality of electrochemical research. An integrated and standardized solution is urgently needed to meet the increasingly sophisticated research needs. Summary of the Invention

[0003] To address the aforementioned shortcomings of existing technologies, this invention aims to provide a constant-temperature electrochemical constant-voltage electrolysis device and testing method. Its core lies in modular integration and a unified constant-temperature design, thus combining compact structure, excellent sealing, and convenient operation. The technical solution adopted by this invention to overcome its shortcomings is as follows: One aspect of the present invention is to provide a constant-temperature electrochemical constant-voltage electrolysis device, comprising: Electrolytic cell body, electrode system, sealing system and electrochemical workstation; The main body of the electrolytic cell includes a double cylindrical glass container, a connection system, a ventilation system, and a constant temperature system; The electrode system includes a working electrode (1), a reference electrode (2), and a counter electrode (3); The sealing system includes a ground joint sealing assembly and an electrode sealing assembly; The electrolytic cell body, electrode system, sealing system and electrochemical workstation together constitute the electrolysis device; the working electrode (1), reference electrode (2) and counter electrode (3) in the electrode system are all connected to the electrochemical workstation through wires. Preferably, the double-cylindrical glass container is made of high borosilicate glass and has a closed bottom and open top structure, including a left-side cavity A and a right-side cavity B; the overall height of the double-cylindrical glass container is 10-15 cm; wherein, the inner radius of the left-side cavity A is 3-5 cm, and the inner radius of the right-side cavity B is 1.5-3 cm; the top of the left-side cavity A is provided with three "19 / 22" standard ground joints, and the top of the right-side cavity B is provided with one "19 / 22" standard ground joint. Preferably, the connection system includes a cylindrical channel located between the bottom regions of the left region A cavity and the right region B cavity, with an inner radius of 1 to 2 cm, and a G3 sand core partition (5) is installed inside the cylindrical channel (4). In the technical solution of the present invention, the connection system includes a cylindrical channel located between the bottom regions of the left region A cavity and the right region B cavity. A G3 sand core partition is installed in the cylindrical channel. The partition allows the solution between the two cavities to be ion-conducting but physically isolated, which can effectively prevent cross-contamination of reaction products between the two electrode regions and ensure the continuous smooth flow of the electrolysis circuit and the high efficiency of the reaction. Preferably, the ventilation system includes a horizontal ventilation channel (6) connecting the upper part of the left region A cavity and the right region B cavity, with an inner radius of 1 to 2 cm; an exhaust channel (7) disposed in the middle of the horizontal ventilation channel (6); and an air intake channel (8) disposed inside the left region A cavity and connected to its top; the air intake channel (8) is a tube made of high borosilicate glass, with the upper end of the air intake pipe passing through and sealed in the top sealing plug, and simultaneously sealed in the ground joint. In the technical solution of this invention, the ventilation system includes a horizontal ventilation pipe connecting the upper parts of the left-side region A cavity and the right-side region B cavity, an exhaust pipe located in the middle of the pipe, and an air intake channel located in the left-side cavity and connected to the top. The upper end of the air intake channel passes through and is sealed and fixed within the top sealing plug and ground joint. This structure constitutes a highly efficient air pressure buffer circuit, which can significantly reduce the pressure shock caused by air intake, achieve a smooth transition and dynamic balance of pressure within the cavity, and ensure that the reaction takes place in a stable atmosphere. Preferably, the constant temperature system includes an external constant temperature circulation device, which is connected to the constant temperature cavity of the electrolysis device through a circulation pipeline. In the technical solution of the present invention, the constant temperature system includes an external constant temperature circulation device, which is connected to the constant temperature cavity of the electrolysis device through a circulation pipeline, thereby forming a closed circulation loop and providing a precise and stable constant temperature environment for the electrolysis process. Preferably, the electrode system includes a working electrode (1), a reference electrode (2), and a counter electrode (3), wherein the working electrode (1) and the reference electrode (2) are both fixed in the cavity of the left region A, and the counter electrode (3) is fixed in the cavity of the right region B; the working electrode (1) and the counter electrode (3) are respectively sealed and installed through a standard ground joint interface, and their upper lead wires pass through the sealing plug and are sealed and fixed in the ground joint; the reference electrode (2) is placed in an independent salt bridge, which includes a high borosilicate glass tube and a porous ceramic core fixed at its bottom as a liquid junction, and its upper end passes through the sealing plug and is sealed and fixed in the ground joint. In the technical solution of this invention, the electrode system includes a working electrode (1), a reference electrode (2), and a counter electrode (3). To reduce interference between electrodes and optimize the electric field distribution, the working electrode and the reference electrode are jointly disposed in cavity A in the left region, while the counter electrode is independently disposed in cavity B in the right region. Both the working electrode and the counter electrode use a standard ground joint interface to achieve a sealed connection with the cavity, and their upper lead wires pass through and are sealed and fixed in the ground joint; the reference electrode is placed in an independent salt bridge, which uses a standard ground joint interface to achieve a sealed connection with the cavity, and the upper end of the salt bridge tube passes through and is sealed and fixed in the ground joint, while its bottom end forms a liquid junction through a porous ceramic core. Preferably, the sealing system includes a ground joint sealing assembly, an electrode sealing assembly, and an air intake channel sealing assembly; the ground joint sealing assembly mates with the ground joint connection structure of the double cylindrical glass container; the electrode sealing assembly and the air intake channel sealing assembly are integrated within the ground joint sealing assembly; the electrode sealing assembly is used to seal and fix the leads of the working electrode and the reference electrode, as well as the salt bridge tube of the reference electrode, respectively, within the ground joint sealing assembly; the air intake channel sealing assembly is used to seal and fix the tube body of the air intake channel within the ground joint sealing assembly. In the technical solution of this invention, the sealing system includes a ground joint sealing assembly, an electrode sealing assembly, and an air inlet channel sealing assembly. The ground joint sealing assembly mates with the "19 / 22" standard ground joint of the double-cylindrical glass container to achieve a static seal of the main body of the reaction chamber. The electrode sealing assembly and the air inlet channel sealing assembly are integrated into the ground joint sealing assembly, forming an auxiliary seal that reliably fixes the working electrode lead, counter electrode lead, salt bridge tube, and air inlet pipe penetration. These components together constitute an integrated sealing module, providing comprehensive airtight protection for the entire electrolysis system. Preferably, the working electrode is selected from any one of platinum, gold, silver, copper, iron, zinc, aluminum, titanium, and nickel, and a glassy carbon electrode, with a thickness of 0.5 to 1.0 mm and a diameter of 10 to 50 mm; the reference electrode is selected from any one of a saturated calomel electrode, a silver / silver chloride electrode, or a mercury / mercury oxide electrode; and the counter electrode is selected from any one of a platinum electrode, a graphite electrode, a titanium electrode, or a carbon rod electrode. In the technical solution of this invention, the working electrode can be selected according to the testing mode: when performing constant voltage electrolysis, it is preferably a sheet structure with a thickness of 0.5~1.0 mm and a diameter of 10~50 mm, and the material is selected from platinum, gold, silver, copper, iron, zinc, aluminum, titanium or nickel, more preferably platinum; when it is necessary to determine the electrolysis potential window by cyclic voltammetry, a glassy carbon electrode is more preferably used. This modular electrode selection scheme allows a single device to be flexibly adapted to both analytical and preparative testing modes, combining versatility and convenience. The reference electrode is selected from saturated calomel electrode, silver / silver chloride electrode or mercury / mercury oxide electrode, more preferably saturated calomel electrode. The counter electrode is selected from platinum electrode, graphite electrode, titanium electrode or carbon rod electrode, more preferably platinum electrode. Preferably, the ground joint sealing assembly is selected from either a polytetrafluoroethylene (PTFE) sealing plug or a rubber sealing plug; the PTFE sealing plug or rubber sealing plug is matched with the ground joint connection structure of the double cylindrical glass container; the electrode sealing assembly and the air inlet channel sealing assembly are selected from either a PTFE sealing strip or a PTFE sealing sleeve. In the technical solution of this invention, the ground joint sealing assembly is selected from either a polytetrafluoroethylene (PTFE) sealing plug or a rubber sealing plug. The PTFE sealing plug or rubber sealing plug is matched with the ground joint connection structure of the double cylindrical glass container to achieve a reliable seal. More preferably, a PTFE sealing plug with better chemical stability is used. The electrode sealing assembly and the air inlet channel sealing assembly are selected from either a PTFE sealing tape or a PTFE sealing sleeve, and are used to achieve a reliable seal at the penetration points of the electrode leads, salt bridge tube, and air inlet pipe. Another object of the present invention is to provide a testing method based on the aforementioned isothermal electrochemical constant voltage electrolysis device.

[0004] S1: Electrolyte preparation and addition: Add a predetermined volume of electrolyte to the main body of the electrolytic cell; S2: System assembly and connection: The working electrode, reference electrode, and counter electrode are installed and fixed using the ground joint sealing assembly and electrode sealing assembly, and then connected to the corresponding interfaces of the electrochemical workstation using wires; at the same time, the air inlet channel is installed and fixed using the ground joint sealing assembly and air inlet channel sealing assembly. S3: Establishment of inert environment and sample loading: Start the constant temperature system and ventilation system and introduce inert gas (such as high-purity nitrogen or argon); under the continuous protection of the inert atmosphere, add the sample to be tested into the electrolyte to establish a stable oxygen-free constant temperature reaction system; S4: Electrochemical Test Execution and Analysis: Set parameters on the electrochemical workstation to perform electrochemical characteristic analysis or constant voltage electrolysis reaction of the sample to be tested. Preferably, in process S1, the electrolyte comprises a supporting electrolyte and an organic solvent; the supporting electrolyte is selected from one of tetrabutylammonium perchlorate (TBAP), tetrabutylammonium hexafluorophosphate (TBAPF6), or tetraethylammonium tetrafluoroborate (TEABF4); the organic solvent is selected from one of benzonitrile (PhCN), acetonitrile (ACN), N,N-dimethylformamide (DMF), or tetrahydrofuran (THF). Preferably, in process S1, the electrolyte is more preferably a combination of tetrabutylammonium perchlorate (TBAP) and benzonitrile (PhCN). In this combination, TBAP dissociates into TBA when dissolved in PhCN solvent. + Cations and ClO4 - Anions effectively reduce the ohmic resistance of the electrolyte system, ensuring efficient current transmission. At the same time, this ionic environment helps to more effectively concentrate the electric field onto the working electrode surface, thereby driving and achieving the desired specific potential response. The advantages and beneficial effects of this invention are as follows: 1. The dual sealing design, consisting of a ground joint and a dedicated sealing component, effectively prevents electrolyte leakage and evaporation.

[0005] 2. The electrode system supports quick replacement. The working electrode can be flexibly selected from glassy carbon electrodes or various metal electrodes according to the test purpose (such as cyclic voltammetry or constant voltage electrolysis), which takes into account both analytical sensitivity and electrolysis stability.

[0006] 3. The device adopts an integrated and modular design with fixed electrode spacing, making it easy to operate and fundamentally improving the repeatability of experiments and the comparability of data.

[0007] 4. The main body is made of high-transmittance glass, which facilitates real-time observation of the electrolyte state, reaction phenomena such as bubble generation or deposit changes on the electrode surface.

[0008] 5. By connecting the left and right cavities through the G3 sand core partition, cross-contamination of reaction products between the two electrode regions is effectively prevented while ensuring ion conduction, thus ensuring the intrinsic nature of the reaction study and the accuracy of the results. Attached Figure Description

[0009] Figure 1 This is a schematic diagram of the overall structure of the isothermal electrochemical constant-voltage electrolysis device described in this invention; Figure 2 This is a cyclic voltammetry (CV) curve measured to determine the optimal electrolysis potential before constant voltage electrolysis is performed on the device in Example 1. Figure 3 This is a time-coulomb curve (the relationship between the electrolytic charge Q and time t) recorded during constant-voltage electrolysis at a determined potential in Example 1. Figure 4 In Example 1, to characterize the electrochemical state of the system after the reaction, the cyclic voltammetry (CV) curves were obtained immediately after constant voltage electrolysis in the same device. Detailed Implementation

[0010] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the following embodiments are for illustrative purposes only and do not constitute a limitation on the scope of protection of this invention. like Figure 1 The diagram shown is a schematic representation of a specific embodiment of the isothermal electrochemical constant-voltage electrolysis device of the present invention. The electrolysis apparatus includes the following components: The main body of the electrolytic cell is a double-cylindrical glass container, closed at the bottom and open at the top. The container is made of high borosilicate glass and has an overall height of 12 cm. The double-cylindrical glass container includes a left-side cavity A and a right-side cavity B. The inner radius of cavity A is 5 cm, and the inner radius of cavity B is 2 cm. The top of cavity A in the left area has three "19 / 22" standard ground joints, and the top of cavity B in the right area has one "19 / 22" standard ground joint, which are used for the installation of the ground joint sealing assembly, the electrode sealing assembly and the air intake channel sealing assembly. The connection system includes a cylindrical channel (4) located at the bottom of cavity A in the left region and cavity B in the right region. A G3 sand core partition (5) is fixedly installed in the channel to achieve ion conduction and physical isolation of the solution between the two cavities; The ventilation system includes: a horizontal ventilation channel (6) connecting the upper part of the left and right cavities; an exhaust channel (7) located in the middle of the horizontal ventilation channel; and an intake channel (8) located inside the left region A cavity and connected to its top, with its upper end passing through the top sealing plug and forming a sealed fixation, and the whole assembly installed in the corresponding ground joint. This structure is used to introduce gas and buffer pressure fluctuations within the cavity; The constant temperature system includes an external constant temperature circulation device (such as a circulating water pump and a constant temperature water tank), which is connected to the constant temperature cavity of the electrolysis device through a circulation pipeline to form a closed loop, so as to achieve precise temperature control of the reaction process. The electrode system includes a working electrode (1), a reference electrode (2), and a counter electrode (3). The working electrode (1) and the reference electrode (2) are installed and fixed in the cavity in the left region A, and the counter electrode (3) is installed and fixed in the cavity in the right region B, thereby reducing interference between electrodes and optimizing the electric field distribution. The working electrode (1) and the counter electrode (3) are sealed to the cavity using a standard ground joint interface, and their upper leads are inserted through a sealing plug and sealed and fixed inside the ground joint. The reference electrode (2) is placed in an independent salt bridge, which is sealed to the cavity using a standard ground joint interface. Its upper end is inserted through a sealing plug and sealed and fixed inside the ground joint, and its bottom end forms a liquid junction through a porous ceramic core. The sealing system includes a ground joint sealing assembly, an electrode sealing assembly, and an air inlet channel sealing assembly. The ground joint sealing assembly mates with the "19 / 22" standard ground joint structure on the top of the container cavity to achieve the main seal of the cavity; the electrode sealing assembly and the air inlet channel sealing assembly are integrated into the ground joint sealing assembly to form an auxiliary seal that reliably fixes the working electrode lead, the counter electrode lead, the salt bridge tube, and the air inlet pipe through-piece. Special Note: In the following embodiments, unless otherwise specified, the term "electrolysis apparatus" refers to... Figure 1 The device with the structure shown.

[0011] In the following embodiments, "adding N molar equivalents of a certain drug" means that the amount of the drug added is the fullerene C added in that embodiment. 60 N times the amount of substance. Example

[0012] Experimental conditions: This embodiment uses a CHI630B electrochemical workstation. The scan rate for cyclic voltammetry was set to 100 mV / s. The electrolyte was a 0.1 M tetrabutylammonium perchlorate (TBAP) solution in benzonitrile (PhCN).

[0013] The electrodes used in the test are as follows: Cyclic voltammetry test: The working electrode is a glassy carbon electrode; the reference electrode is a saturated calomel electrode; the counter electrode is a rolled platinum sheet electrode with a thickness of 0.5 mm and a diameter of 50 mm.

[0014] Constant voltage electrolysis: The working electrode is replaced with a rolled platinum sheet electrode of the same specifications as the counter electrode, while the reference electrode and the counter electrode remain unchanged.

[0015] Before and throughout the experiment, high-purity nitrogen (N2) was continuously introduced into the electrolytic cell to completely remove and isolate oxygen, ensuring that the experiment was conducted in an inert atmosphere.

[0016] The following theoretical electric charge is calculated based on Faraday's law: Q = n*N*F, where n is the number of electrons transferred, N is the amount of substance of the reactant, and F is the Faraday constant. The specific steps are as follows: S1: Electrolyte preparation and addition.

[0017] This step specifically includes the following sequential operations: 1. Electrolyte preparation: Accurately weigh 8.54 g of tetrabutylammonium perchlorate (TBAP), place it in a 250 mL volumetric flask, dissolve it with benzonitrile (PhCN) and make up to volume to obtain a TBAP / PhCN electrolyte with a concentration of 0.1 mol / L.

[0018] 2. Volume Calculation and Safety Confirmation: Based on the device dimensions (Area A: inner radius 5 cm, height 12 cm; Area B: inner radius 2 cm, height 12 cm), to ensure operational safety and allow sufficient space, the electrolyte level in each chamber should be controlled within 2 / 3 of its total height (i.e., ≤8 cm). Calculations show that the maximum effective volume corresponding to this level is significantly larger than the total volume of the 250 mL electrolyte prepared in this step; therefore, it can be safely injected.

[0019] 3. Solution addition: Electrolyte is injected into chambers A and B respectively. The liquids in the two chambers are connected through the bottom G3 sand core partition, and the liquid level quickly reaches equilibrium under the action of hydrostatic pressure, thereby ensuring that both electrode areas are submerged. S2: System assembly and connection.

[0020] This step specifically includes the following sequential operations: Lead pretreatment and sealing preparation: First, ensure that the surfaces of the lead-through sections of the working electrode, reference electrode, and counter electrode are clean and dry. Then, take PTFE sealing tape and apply it evenly and smoothly to the corresponding parts of the working electrode lead, counter electrode lead, salt bridge tube, and inlet tube in a spiral manner consistent with the screw-in direction of the sealing plug (clockwise) to form a pre-sealed body.

[0021] 2. Electrode and Vent Pipe Sealing Installation: Pass the working electrode lead, counter electrode lead, salt bridge tube, and inlet tube, already wrapped with sealing tape, sequentially through the center holes of their respective PTFE sealing plugs. Then, align each sealing plug with the corresponding standard ground joint on the top of the device and screw them in together. Upon tightening, the inner wall of the sealing plug exerts uniform radial pressure on the sealing tape, ensuring it fully fills the gaps between the leads, tubes, and plug holes, thus achieving reliable axial and radial sealing. Finally, ensure that each lead and tube passes through the sealing plug from the top and is securely fixed within the ground joint. Afterward, place the reference electrode in the salt bridge and add an appropriate amount of saturated KCl aqueous solution.

[0022] 3. Electrode Connection: After all electrodes have been sealed and fixed as described above, use dedicated wires to connect the working electrode, reference electrode, and counter electrode to the working electrode (WE), reference electrode (RE), and counter electrode (CE) interfaces of the electrochemical workstation, respectively, to complete the construction of the test circuit. S3: Establishment of inert environment and sample loading.

[0023] This step specifically includes the following sequential operations: 1. Establishing an inert environment: Start the constant temperature system to control the system temperature at 25 ℃; at the same time, start the ventilation system to continuously introduce high-purity nitrogen (N2) into the device to maintain an oxygen-free and constant-temperature reaction atmosphere.

[0024] 2. Sample introduction: Under the protection of continuous N2 flow, accurately weigh 500 mg of fullerene C. 60 Briefly open the sealed ground joint, quickly transfer it to cavity A, and stir it thoroughly to disperse it evenly. S4: Electrochemical test execution and analysis.

[0025] This step specifically includes the following continuous operations and analysis processes: 1. Determination of electrolysis potential: Under the same system conditions (including electrolyte, temperature, and atmosphere) as the subsequent constant-voltage electrolysis, the electrolysis potential of fullerene C was first determined using cyclic voltammetry. 60 Perform an electrochemical scan. For example... Figure 2 As shown, the CV curve clearly presents C 60 The characteristic redox peaks of [the substance]. Based on this, in order to obtain the fullerene divalent anion (C [the substance]), 60 2- The optimal reduction potential for subsequent constant voltage electrolysis was determined to be -1.1 V.

[0026] Constant-voltage electrolysis process: At a predetermined potential of -1.1 V, a constant voltage is applied to the system for electrolytic reduction, and the reaction progress is controlled by real-time monitoring of the accumulated charge. Electrolysis is terminated when the total electrolytic charge reaches 140.4 C (slightly higher than the theoretical charge of 134 C calculated based on the stoichiometry of the reaction) and the electrolytic current decreases significantly and tends to stabilize. This indicates that the target reduction reaction has been substantially completed according to stoichiometry, and the slightly excess charge applied ensures the complete completion of the reaction.

[0027] Characterization of the system state after electrolysis: Immediately after the electrolysis reaction was completed, in-situ cyclic voltammetry was performed in the original apparatus to examine the electrochemical behavior of the system after the reaction. The obtained cyclic voltammetry curves are shown below. Figure 4 As shown. At an applied potential of –1.1 V, the response current approaches zero, indicating that the system has reached electrochemical steady state. No net electron transfer occurs at this potential, confirming the neutral fullerene C2.60 It has been completely reduced to fullerene divalent anions (C 60 2- ). The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the claims.

Claims

1. A thermostatic electrochemical constant potential electrolysis device, characterized by, The electrolytic device comprises an electrolytic cell body, an electrode system, a sealing system and an electrochemical workstation. The electrolytic cell body comprises a double-cylinder glass container, a connecting system, a ventilation system and a constant temperature system. The electrode system comprises a working electrode (1), a reference electrode (2) and a counter electrode (3). The sealing system comprises a ground-in sealing assembly and an electrode sealing assembly. The electrolytic device is composed of the electrolytic cell body, the electrode system, the sealing system and the electrochemical workstation. The double-cylinder glass container is made of high borosilicate glass and has a closed bottom and an open top, comprising a left side area A cavity and a right side area B cavity.

2. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The double-cylinder glass container has a total height of 10-15 cm.

3. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The left side area A cavity has an inner radius of 3-5 cm, and the right side area B cavity has an inner radius of 1.5-3 cm.

4. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The left side area A cavity is provided with three "19 / 22" standard ground-in openings at the top, and the right side area B cavity is provided with one "19 / 22" standard ground-in opening at the top.

5. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The connecting system comprises a cylindrical channel between the bottom areas of the left side area A cavity and the right side area B cavity, with an inner radius of 1-2 cm.

6. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The ventilation system comprises a horizontal ventilation channel (6) connecting the upper parts of the left side area A cavity and the right side area B cavity, with an inner radius of 1-2 cm. The ventilation system further comprises an exhaust channel (7) arranged in the middle of the horizontal ventilation channel (6) and an air inlet channel (8) arranged in the left side area A cavity and communicating with the top thereof. The air inlet channel (8) is a pipe body made of high borosilicate glass, with the upper end penetrating and sealingly fixed in the sealing plug at the top and sealingly fixed in the ground-in opening. The constant temperature system comprises an external constant temperature circulating device connected to the constant temperature cavity of the electrolytic device through a circulating pipeline. The electrode system comprises a working electrode (1), a reference electrode (2) and a counter electrode (3), wherein the working electrode (1) and the reference electrode (2) are fixed in the left side area A cavity, and the counter electrode (3) is fixed in the right side area B cavity. The working electrode (1) and the counter electrode (3) are sealingly installed through standard ground-in opening interfaces, with the upper end lead penetrating and sealingly fixed in the sealing plug and the ground-in opening. The reference electrode (2) is arranged in an independent salt bridge comprising a high borosilicate glass pipe body and a porous ceramic core as a liquid connection part fixed at the bottom end, with the upper end penetrating and sealingly fixed in the sealing plug and the ground-in opening.

7. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The sealing system comprises a ground joint sealing assembly, an electrode sealing assembly and an air inlet channel sealing assembly; the ground joint sealing assembly is matched with a ground joint connecting structure of the double-cylinder glass container; the electrode sealing assembly and the air inlet channel sealing assembly are integrated in the ground joint sealing assembly; the electrode sealing assembly is used for sealing and fixing the lead wires of the working electrode and the reference electrode and the salt bridge tube of the reference electrode in the ground joint sealing assembly; and the air inlet channel sealing assembly is used for sealing and fixing the tube body of the air inlet channel in the ground joint sealing assembly.

8. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The working electrode (1) is selected from any one of platinum, gold, silver, copper, iron, zinc, aluminum, titanium and nickel, and a glassy carbon electrode with a thickness of 0.5-1.0 mm and a diameter of 10-50 mm; the reference electrode (2) is selected from any one of a saturated calomel electrode, a silver / silver chloride electrode or a mercury / mercury oxide electrode; and the counter electrode (3) is selected from any one of a platinum electrode, a graphite electrode, a titanium electrode or a carbon rod electrode.

9. The thermostatic electrochemical constant potential electrolysis device according to claim 1, characterized in that: The ground joint sealing assembly is selected from any one of a polytetrafluoroethylene sealing plug or a rubber sealing plug; the polytetrafluoroethylene sealing plug or the rubber sealing plug is matched with the ground joint connecting structure of the double-cylinder glass container; and the electrode sealing assembly and the air inlet channel sealing assembly are selected from any one of a polytetrafluoroethylene sealing strip or a polytetrafluoroethylene sealing sleeve.

10. The method of testing of claim 1, wherein, The specific steps are as follows: S1: electrolyte configuration and addition: adding a predetermined volume of electrolyte into the electrolytic cell body; S2: system assembly and connection: installing and fixing the working electrode, the reference electrode and the counter electrode through the ground joint sealing assembly and the electrode sealing assembly, and then connecting the three to the corresponding interfaces of the electrochemical workstation through wires; at the same time, installing and fixing the air inlet channel through the ground joint sealing assembly and the air inlet channel sealing assembly; S3: establishment of inert environment and sample loading: starting the constant temperature system and the aeration system to introduce inert gas (such as high-purity nitrogen or argon); under the protection of continuous inert atmosphere, adding the sample to be tested into the electrolyte, so as to establish a stable anaerobic constant temperature reaction system; S4: electrochemical test execution and analysis: setting parameters on the electrochemical workstation to perform electrochemical characteristic analysis or constant voltage electrolysis reaction of the sample to be tested.

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