In-situ monitoring method for reaction stability of titanium-containing multiphase electrode in electrolysis process

Abstract

The invention discloses an in-situ monitoring method for reaction stability of a titanium-containing multiphase electrode in an electrolysis process, and belongs to the field of electrochemical metallurgy. On the basis of the closed gas sensor detection chamber, through gas circuit connection with the molten salt electrolysis furnace, real-time in-situ monitoring of gas production components and concentration in the electrolysis process is realized, so that the specific reaction condition is judged. And the argon bottle, the pressure reducing valve, the flowmeter, the high-temperature molten salt resistance furnace, the water cooling device and the gas detection cabin are connected with the safety bottle and the tail gas bottle through polytetrafluoroethylene hoses. According to the method, the quantitative relation among the gas volume signal, the electrolysis overpotential and the electrode surface area is established, the change of the electrode surface area in the electrolysis process is calculated and analyzed in real time, the electrolysis system is regulated and controlled by adjusting the electrode surface area, inputting the current density and the like to recover stability, and the reason of the change of the electrolysis overpotential is analyzed; and in-situ monitoring of the reaction stability of the titanium-containing multiphase electrode in the electrolysis process is realized. The electrolysis environment is consistent with the commercial titanium molten salt electrolysis environment.

Description

An in-situ monitoring method for reaction stability in the electrolysis process using titanium-containing multiphase electrodes Technical Field

[0001] This invention relates to an in-situ detection method for the carbon-containing anodic dissolution reaction process, belonging to the field of electrochemical metallurgy technology. Background Technology

[0002] Titanium metal possesses advantages such as low density, high specific strength, and corrosion resistance. In the existing utilization processes of my country's unique vanadium-titanium magnetite, titanium is mainly found in high-titanium slag from electric furnaces and titanium-containing blast furnace slag. However, the titanium extraction process from high-titanium slag suffers from low utilization rates, heavy pollution, and a long process: due to the high content of impurities such as CaO and MgO, Panzhihua titanium slag cannot be directly used in the fluidized bed chlorination process to produce sponge titanium; it can only be used as a raw material for the sulfuric acid process to produce titanium dioxide.

[0003] In recent years, researchers have focused on preparing metallic titanium and its alloys from titanium oxides via molten salt electrolysis, avoiding chlorination processes and offering a shorter process flow. Among these methods, the soluble anodic electrolytic extraction of titanium (USTB method) is currently recognized as a molten salt electrolytic titanium extraction method with significant industrial potential. Its principle involves using a titanium carbon-oxygen solid solution (TiC). x O y The cathode is used as a soluble anode for electrolysis. Titanium enters the molten salt as divalent or trivalent ions and is deposited at the cathode, while carbon and oxygen escape as carbon monoxide (CO) or carbon dioxide (CO2).

[0004] The composition of the gas produced in the reaction is directly related to the morphology of the anode byproducts. When the carbon-to-oxygen ratio (molar ratio) of the carbon-containing anode is higher than 1, the anode byproducts are carbon black and CO2. As the reaction proceeds, the carbon black floats on the molten salt surface, posing a risk of short circuit. When the carbon-to-oxygen ratio of the carbon-containing anode is lower than 1, the anode byproduct is titanium oxide. Since titanium oxide is an insulator, it reduces the effective reaction area on the anode surface, and may even prevent the electrolysis reaction from proceeding. Theoretically, when the carbon-to-oxygen ratio is 1, anode dissolution only produces CO, with no other side reactions. However, due to the complex distribution of electrode components and uneven overpotential distribution, the actual reaction situation is more complex. Furthermore, due to the harsh conditions of high-temperature molten salt electrolysis and the complexity of electrode components, in-situ detection of the carbon-containing anode dissolution process remains challenging. Therefore, developing an in-situ detection method for the carbon-containing anode dissolution process from the perspective of gas production is of great significance for the detection and stabilization of the titanium production electrolysis process. Summary of the Invention

[0005] To address the challenge of in-situ detection of carbon-containing anodic dissolution reactions in existing methods, this invention aims to provide an in-situ monitoring method for the reaction stability of titanium-containing multiphase electrode electrolysis processes. This method employs an in-situ detection approach based on gas composition, enabling real-time in-situ monitoring of the composition and concentration of generated gases during electrolysis. It establishes a correlation between the electrolysis process and gas components, and adjusts electrolysis parameters such as current density based on this correlation to monitor the system's reaction process, reaction rate, and stability, thereby achieving stable electrochemical extraction. The in-situ monitoring device for the reaction stability of titanium-containing multiphase electrode electrolysis processes provided by this invention is easy to operate, and the electrolysis environment is consistent with that of commercial titanium molten salt electrolysis, ensuring complete and accurate test results.

[0006] To achieve the above objectives, the present invention adopts the following solution:

[0007] This invention discloses an in-situ method for monitoring the reaction stability of a titanium-containing multiphase electrode electrolysis process, comprising the following steps:

[0008] Step 1: Connect the argon cylinder, pressure reducing valve, flow meter, high-temperature molten salt resistance furnace, water cooling device, gas detection chamber, safety cylinder, and tail gas cylinder via PTFE tubing. The CO gas sensor, CO2 gas sensor, and temperature sensor are embedded inside the enclosed gas sensor detection chamber and connected to a computer for data acquisition and analysis via sensor data acquisition lines. During operation, high-purity argon gas is continuously supplied through the high-purity argon cylinder. The computer controls the electrolysis current and collects the electrolysis voltage change signal. The CO and CO2 gases produced by the reaction are blown out from the high-temperature molten salt resistance furnace, cooled by the water cooling gas path, and then enter the enclosed gas sensor detection chamber. The CO and CO2 gas sensors detect the volume fraction signals of CO and CO2 gases, and the temperature sensor detects the gas temperature signal to prevent damage to the sensors due to high temperatures. The gas volume fraction signal, electrolysis voltage change signal, and gas temperature signal are collected together in the computer for further analysis. The gas flows into the tail gas cylinder, is treated, and then released into the atmosphere.

[0009] Step 2: Based on the collected real-time gas volume fraction signals c of CO and CO2, obtain the gas generation rate (N) and the gas change rate. The gas generation rate is calculated using the following formula:

[0010]

[0011] Where N is the gas production rate, in mol / s. Q is the gas flow rate, in ml / s. c is the gas volume fraction, dimensionless. V m The standard gas constant is expressed in mol / L. The rate of change of gas volume fraction is obtained by differentiating N with respect to time t.

[0012] When the gas production rate is stable, it indicates that the system is in a stable electrolysis state.

[0013] This indicates that the anolyte current density / overpotential has increased, leading to an increased gas production rate. The system can be brought back to a stable state by increasing the electrode reaction surface area or decreasing the external current density.

[0014] When this occurs, it indicates a decrease in anolyte current density / overpotential, leading to a reduction in gas production rate. The system can be brought back to a stable state by reducing the electrode reaction surface area or increasing the external current density.

[0015] Step 3: Establish the gas volume fraction C o The relationship between the overpotential η and the current at time t1 and time t2 is equal. The change in gas production rate has a quantitative relationship with the change in electrode overpotential:

[0016]

[0017] Where F is the Faraday constant, and A t1 A t2 The anode surface areas at times t1 and t2 are shown in m². 2 C O (0,t1) and C O (0, t2) represent the oxide concentrations at the anolyte interface at times t1 and t2, respectively, in megohms (M). α represents the electrode reaction transfer coefficient. η t1 With η t2 t1 and t2 are the anodic overpotentials at times t1 and t2, respectively, in V. R is the gas constant, and T is the temperature in K. R (0,t1),C R (0, t2) represent the concentrations of the reductant at the anolyte interface at times t1 and t2, respectively, in megohms (M). Simplifying the above equation yields:

[0018]

[0019] Step four: Obtain the gas change rate and the gas volume fraction change acceleration by differentiating the gas production rate N with respect to time t. There is a quantitative relationship among them:

[0020]

[0021] Substituting these values ​​into the final equation obtained in step three, we get the following formula:

[0022]

[0023] The effects of electrode area variation on gas production and overpotential are quantitatively analyzed using the above relationships. The anode overpotential η at times t1 and t2 is obtained from the electrolysis voltage change signal. t1 With η t2 The anode surface area A at time t1 and time t2 is obtained. t1 With A t2 The input current density is then adjusted based on the change in anode surface area, satisfying the following relationship:

[0024] A t1 j t1 =A t2 j t2

[0025] Where j t1 To regulate the current density before, j t2 The current density after adjustment is expressed in A / cm². 2 By feeding back the gas volume fraction signal to adjust the input current density for a total time not exceeding 40 seconds, in-situ monitoring of the reaction stability during the electrolysis process of titanium multiphase electrodes can be achieved.

[0026] Furthermore, the gas sensors include, but are not limited to, carbon dioxide gas sensors, methane gas sensors, and carbon monoxide gas sensors.

[0027] Furthermore, the method can be applied to any electrochemical system exhibiting carbon-containing anode gas generation behavior, including but not limited to aqueous solution systems, room-temperature ionic liquid systems, and high-temperature molten salt electrochemical systems.

[0028] Furthermore, the method is based on the quantitative analysis of gas concentration and change rate obtained from in-situ observation by gas sensing, to establish the quantitative relationship between cell voltage change, gas concentration and its change rate, reaction rate, and reaction process, and to quantitatively characterize the stability of the electrolysis system through the gas concentration change rate, thus constructing an in-situ control method.

[0029] This invention discloses an in-situ monitoring device for the reaction stability of a titanium-containing multiphase electrode electrolysis process, used to implement the aforementioned in-situ monitoring method for the reaction stability of a titanium-containing multiphase electrode electrolysis process. The device includes a high-purity argon cylinder, a pressure reducing valve, a flow meter, a resistance furnace chamber, a resistance furnace cover, electrodes, a vacuum valve, a vacuum pump, an exhaust valve, a water cooling device, a gas detection chamber, a data acquisition and analysis computer, a safety bottle, and a tail gas bottle. The high-purity argon cylinder, pressure reducing valve, flow meter, resistance furnace chamber, exhaust valve, water cooling device, gas detection chamber, safety bottle, and tail gas bottle are connected via polytetrafluoroethylene (PTFE) flexible hoses.

[0030] Furthermore, the gas detection chamber includes a top cover lead hole, a gas detection chamber body, a flange, a chamber air inlet, a chamber air outlet, a CO gas sensor, a CO2 gas sensor, a temperature sensor, and sensor data acquisition lines. The sensor data acquisition lines are connected to the sensors through the top cover lead hole and sealed by the flange. The data from the CO gas sensor, CO2 gas sensor, and temperature sensor are aggregated in real time to the data acquisition and analysis computer via the data acquisition lines.

[0031] Furthermore, the temperature sensor is connected to the chip and transmits data to the receiver wirelessly, while the gas sensor transmits data to the receiver via wired connection, allowing direct reading of the measured temperature, pressure, and gas concentration data.

[0032] Beneficial effects:

[0033] 1. This invention discloses a method and apparatus for in-situ monitoring of reaction stability during the electrolysis process of titanium-containing multiphase electrodes. Based on a closed gas sensor detection chamber, it is connected to the gas path of a molten salt electrolysis furnace to achieve real-time in-situ monitoring of the composition and concentration of gas produced during electrolysis, thereby determining the specific reaction conditions. Compared with optical in-situ detection methods, this invention has no structural requirements on the experimental electrolysis furnace and has the advantages of high safety, simple implementation, accurate measurement, timely response, and non-destructive testing.

[0034] 2. This invention discloses an in-situ monitoring method and device for the reaction stability of a titanium-containing multiphase electrode electrolysis process. Based on the quantitative analysis of gas concentration and change rate obtained from in-situ gas sensing, a quantitative relationship is established between cell voltage change and gas concentration and its change rate. Correlation relationships are established between a series of electrolysis process parameter changes, including anode dissolution and shedding, cathode deposition and dendrite growth, and electrode spatial position changes, and the gas concentration and change rate. Based on these correlation relationships, the change in electrode surface area during the electrolysis process is calculated and analyzed in real time. The electrolysis system is then regulated to restore stability by adjusting the electrode surface area and input current density, and the causes of electrolysis overpotential changes are analyzed, thus achieving in-situ monitoring of the reaction stability of the titanium-containing multiphase electrode electrolysis process.

[0035] 3. The present invention discloses an in-situ monitoring method and device for the reaction stability of a titanium-containing multiphase electrode electrolysis process. Based on the gas generation mechanism of the titanium-containing electrode electrolysis process, an in-situ control method for the electrolysis process is constructed. The electrolysis process is controlled by adjusting the electrode shape and spatial position and regulating the current density. The stability of the reaction process and the control effect are verified by the real-time change of gas concentration.

[0036] 4. The present invention discloses an in-situ monitoring method and device for the reaction stability of a titanium-containing multiphase electrode electrolysis process. By adjusting the gas pressure and temperature of the gas entering the sensor detection chamber through a water cooling device, the monitoring effect is not affected by the temperature, gas pressure, and gas atmosphere of the electrolysis system. It can be applied to any electrochemical system with carbon-containing anode gas generation behavior, including but not limited to aqueous solution systems, room temperature ionic liquid systems, and high temperature molten salt electrochemical systems. Attached Figure Description

[0037] Figure 1 is a schematic diagram of an in-situ gas generation detection device for a titanium-containing electrode electrolysis process according to the present invention.

[0038] Figure 2 is a schematic diagram of the gas detection chamber.

[0039] Figure 3 shows the electrolysis curves and the CO2 gas yield, concentration change, and concentration change acceleration curves of the example.

[0040] Among them: 1-High-purity argon cylinder, 2-Pressure reducing valve, 3-Flow meter, 4-Resistance furnace chamber, 5-Resistance furnace cover, 6-Electrode, 7-Vacuum valve, 8-Vacuum pump, 9-Exhaust valve, 10-Water cooling device, 11-Gas detection chamber, 12-Data acquisition and analysis function computer, 13-Safety bottle, 14-Tail gas bottle, 15-Top cover lead hole, 16-Gas detection chamber body, 17-Flange, 18-Chamber air inlet, 19-Chamber air outlet, 20-CO gas sensor, 21-CO2 gas sensor, 22-Sensor data acquisition line, 23-Temperature sensor. Detailed Implementation

[0041] The present invention will be further described in detail below with reference to the embodiments of titanium carbon oxygen nitrogen anodic electrolysis dissolution gas production and the accompanying drawings. The embodiments of the present invention are not limited thereto.

[0042] As shown in Figure 1, this embodiment discloses an in-situ monitoring device for the reaction stability of a titanium-containing multiphase electrode electrolysis process, comprising 1 high-purity argon cylinder, 2 pressure reducing valve, 3 flow meter, 4 resistance furnace chamber, 5 resistance furnace cover, 6 electrode, 7 vacuum valve, 8 vacuum pump, 9 exhaust valve, 10 water cooling device, 11 gas detection chamber, 12 data acquisition and analysis computer, 13 safety bottle, and 14 tail gas bottle. The above structures are connected by a polytetrafluoroethylene hose for gas path connection. The gas volume fraction signal, electrolysis voltage change signal, and gas temperature signal are all collected to the data acquisition and analysis computer. The gas detection chamber includes 11 (top cover lead hole), 15 (gas detection chamber body), 16 (flange), 17 (chamber air inlet), 18 (chamber air outlet), 19 (chamber air outlet), 20 (CO gas sensor), 21 (CO2 gas sensor), 22 (temperature sensor), and 23 (sensor data acquisition line). The sensor data acquisition line is connected to the sensor through the top cover lead hole and sealed by the flange. The data from the CO gas sensor, CO2 gas sensor, and temperature sensor are aggregated in real time to the data acquisition and analysis computer via the data acquisition line, as shown in Figure 2.

[0043] This embodiment discloses an in-situ method for monitoring the reaction stability of a titanium-containing multiphase electrode electrolysis process. The specific implementation steps are as follows:

[0044] Step 1: Connect the commercial argon cylinder, pressure reducing valve, flow meter, high-temperature molten salt resistance furnace, water cooling device, gas detection chamber, safety cylinder, and tail gas cylinder via PTFE tubing. The CO gas sensor, CO2 gas sensor, and temperature sensor are embedded inside the enclosed gas sensor detection chamber and connected to a computer for data acquisition and analysis via sensor data acquisition lines. During operation, high-purity argon gas is continuously supplied through the high-purity argon cylinder. The computer controls the electrolysis current and collects the electrolysis voltage change signal. The CO and CO2 gases produced by the reaction are blown out from the high-temperature molten salt resistance furnace, cooled by the water cooling gas path, and then enter the enclosed gas sensor detection chamber. The CO and CO2 gas sensors detect the volume fraction signals of CO and CO2 gases, and the temperature sensor detects the gas temperature signal to prevent damage to the sensors due to high temperatures. The gas volume fraction signal, electrolysis voltage change signal, and gas temperature signal are collected together in the computer for further analysis. Finally, the gas flows into the tail gas cylinder, is processed, and then released into the atmosphere.

[0045] Step 2: Based on the collected real-time gas volume fraction signals c of CO and CO2, obtain the gas generation rate (N) and the gas change rate. The gas generation rate is calculated using the following formula:

[0046]

[0047] Where N is the gas production rate, in mol / s; Q is the gas flow rate, in ml / s; c is the gas volume fraction, dimensionless; V m The standard gas constant is expressed in mol / L. The rate of change of gas volume fraction is obtained by differentiating N with respect to time t.

[0048] When the gas production rate is stable, it indicates that the system is in a stable electrolysis state.

[0049] When the anode current density / overpotential increases, the gas production rate increases. At this time, the system can be brought back to a stable state by increasing the electrode reaction surface area or reducing the external current density.

[0050] When the anode current density / overpotential decreases, the gas production rate decreases. At this time, the system can be brought back to a stable state by reducing the electrode reaction surface area or increasing the external current density.

[0051] Step 3: Establish the gas volume fraction C o The relationship between the overpotential η and the current at time t1 and time t2 is equal. The change in gas production rate has a quantitative relationship with the change in electrode overpotential:

[0052]

[0053] Where F is the Faraday constant, and A t1 A t2 The anode surface areas at times t1 and t2 are shown in m². 2 C O (0,t1) and C O (0, t2) represent the oxide concentrations at the anode interface at times t1 and t2, respectively, in units of M; α represents the electrode reaction transfer coefficient; η t1 With η t2 t1 and t2 are the anodic overpotentials at times t1 and t2, respectively, in V; R is the gas constant, T is the temperature, in K; C R (0,t1),C R (0, t2) represent the concentrations of the reductant at the anolyte interface at times t1 and t2, respectively, in megohms (M). Simplifying the above equation yields:

[0054]

[0055] Step four: Obtain the gas change rate and the gas volume fraction change acceleration by differentiating the gas production rate N with respect to time t. There is a quantitative relationship among them:

[0056]

[0057] Substituting these values ​​into the final equation obtained in step three yields the following formula:

[0058]

[0059] The above relationships allow for a quantitative analysis of the impact of electrode area changes on gas production and overpotential. The anode overpotential η at times t1 and t2 is obtained using the electrolysis voltage change signal. t1 With η t2 The anode surface area A at time t1 and time t2 can be obtained. t1 With A t2 The input current density is then adjusted based on the change in anode surface area, satisfying the following relationship:

[0060] A t1 j t1 =A t2 j t2

[0061] Where j t1 To regulate the current density before, j t2 The current density after adjustment is expressed in A / cm². 2 By feeding back the gas volume fraction signal to adjust the input current density for a total time not exceeding 40 seconds, in-situ monitoring of the reaction stability during the electrolysis process of titanium multiphase electrodes can be achieved.

[0062] The anode material system is a 93% titanium-carbon-oxygen solid solution, and the negative electrode is a pure titanium extraction system. The evolution of CO2, CO, and temperature during electrolytic titanium extraction at 550℃ was studied. Before electrolysis, exhaust valve 9 and pressure reducing valve 2 were closed, vacuum valve 7 was opened, and vacuum pump 8 was turned on to evacuate the furnace chamber 4 to a pressure of 0 MPa. Vacuum valve 7 and vacuum pump 8 were then closed, and the mixture was allowed to stand for 5 minutes to ensure good airtightness of the furnace chamber and the gas passages before and after. Pressure reducing valve 2 was opened, and flow meter 3 was adjusted to introduce argon gas into the furnace chamber 4 to 0.1 MPa. Exhaust valve 9 was opened to continuously introduce argon gas, completely purging any remaining air in the gas passages. The furnace was started and heated to 550℃, held for 1 hour, and then CO gas sensor 20, CO2 gas sensor 21, and temperature sensor 23 were activated until the gas readings stabilized. Electrode 6 was connected to data acquisition unit 12 to begin the electrolysis process and continuously record gas reading changes. During electrolysis, a sudden voltage change occurs, as shown in Figure 3, with the voltage rising by 0.5V. Based on the conclusion obtained in step four above, the current density decreases by 0.072 A / cm². 2From the time the signal was emitted to the change in current density, it took 30 seconds. After 10 seconds, the voltage returned to the normal range, indicating that the electrolysis process was stable. This demonstrates that the in-situ monitoring method for the stability of the electrolysis process is effective.

[0063] The method of this invention can be used for quantitative and qualitative analysis of different gas types and concentrations in multi-system and multi-type electrolysis processes. By corresponding the changes in voltage and current curves with changes in temperature, gas pressure, and gas sensor readings during electrolysis, the relationships between temperature, gas pressure, and different gas concentrations as a function of current and voltage can be obtained. This allows for the analysis of gas evolution equations and electrolysis reaction mechanisms at different times and under different conditions.

[0064] The above detailed description further illustrates the purpose, technical solution, and beneficial effects of the invention. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for in-situ monitoring of reaction stability during electrolysis using titanium-containing multiphase electrodes, characterized in that: The process includes the following steps: Step 1: Connect the argon cylinder, pressure reducing valve, flow meter, high-temperature molten salt resistance furnace, water cooling device, gas detection chamber, safety cylinder, and tail gas cylinder via a PTFE hose. The CO gas sensor, CO2 gas sensor, and temperature sensor are embedded inside the enclosed gas sensor detection chamber, and connected to a data acquisition and analysis computer via sensor data acquisition lines. During operation, high-purity argon gas is continuously supplied through the high-purity argon cylinder. The computer controls the electrolysis current and collects the electrolysis voltage change signals. The CO and CO2 gases produced in the reaction are then transferred from the high-temperature molten salt resistance furnace... The gas is blown out of the furnace, cooled by a water-cooled gas path, and then enters a closed gas sensor detection chamber. CO and CO2 gas volume fraction signals are detected by CO and CO2 gas sensors, and the gas temperature signal is detected by a temperature sensor to prevent damage to the sensors due to high temperatures. The gas volume fraction signal, electrolysis voltage change signal, and gas temperature signal are collected together and sent to a computer for further analysis. The gas flows into a tail gas cylinder, is processed, and then released into the atmosphere. Step two: Based on the collected real-time CO and CO2 gas volume fraction signals c, the gas generation rate (N) and gas change rate are obtained. The gas generation rate is calculated using the following formula: Where N is the gas production rate, in mol / s; Q is the gas flow rate, in ml / s; c is the gas volume fraction, dimensionless; V m The standard gas constant is expressed in mol / L; the rate of change of gas volume fraction is obtained by differentiating N with respect to time t. When the gas production rate is stable, it indicates that the system is in a stable electrolysis state. When the anode current density / overpotential increases, the gas production rate increases; the system can be brought back to a stable state by increasing the electrode reaction surface area or decreasing the external current density. When this occurs, it indicates that the anolyte current density / overpotential decreases, leading to a decrease in the gas production rate. The system can be brought back to a stable state by reducing the electrode reaction surface area or increasing the external current density. Step 3: Establish the gas volume fraction C. o The relationship between the overpotential η and the current at time t1 and time t2 is equal under constant current electrolysis conditions. The change in gas production rate has a quantitative relationship with the change in electrode overpotential. Where F is the Faraday constant, and A t1 A t2 The anode surface areas at times t1 and t2 are shown in m². 2 C O (0,t1) and C O (0, t2) represent the oxide concentrations at the anode interface at times t1 and t2, respectively, in units of M; α represents the electrode reaction transfer coefficient; η t1 With η t2 t1 and t2 are the anodic overpotentials at times t1 and t2, respectively, in V; R is the gas constant, T is the temperature, in K; C R (0,t1),C R (0, t2) represent the concentrations of the reductant at the anolyte interface at times t1 and t2, respectively, in units of M; simplifying the above equation yields: Step four: Obtain the gas change rate and the gas volume fraction change acceleration by differentiating the gas production rate N with respect to time t. There is a quantitative relationship among them: Substituting these values ​​into the final equation obtained in step three, we get the following formula: The effects of electrode area changes on gas production and overpotential are quantitatively analyzed using the above relationships; the anode overpotential η at time t1 and t2 is obtained from the electrolysis voltage change signal. t1 With η t2 The anode surface area A at time t1 and time t2 is obtained. t1 With A t2 Furthermore, the input current density is adjusted according to the change in anode surface area, which satisfies the following relationship: A t1 j t1 =A t2 j t2 Where j t1 To regulate the current density before, j t2 The current density after adjustment is expressed in A / cm². 2 The total time for feeding back the gas volume fraction signal to the adjustment input current density does not exceed 40 seconds, thus enabling in-situ monitoring of the reaction stability during the electrolysis process of titanium multiphase electrodes.

2. An apparatus for implementing the method as described in claim 1, characterized in that: It includes a high-purity argon cylinder, a pressure reducing valve, a flow meter, a resistance furnace chamber, a resistance furnace cover, electrodes, a vacuum valve, a vacuum pump, an exhaust valve, a water cooling device, a gas detection chamber, a computer for data acquisition and analysis, a safety cylinder, and a tail gas cylinder. The high-purity argon cylinder, pressure reducing valve, flow meter, resistance furnace chamber, exhaust valve, water cooling device, gas detection chamber, safety cylinder, and tail gas cylinder are connected by polytetrafluoroethylene (PTFE) hoses.

3. The apparatus as described in claim 2, characterized in that: The gas detection chamber includes a top cover lead hole, a gas detection chamber body, a flange, a chamber air inlet, a chamber air outlet, a CO gas sensor, a CO2 gas sensor, a temperature sensor, and sensor data acquisition lines. The sensor data acquisition lines are connected to the sensors through the top cover lead hole and sealed by the flange. The data from the CO gas sensor, CO2 gas sensor, and temperature sensor are aggregated in real time to the data acquisition and analysis computer via the data acquisition lines.

4. The apparatus as described in claim 2 or 3, characterized in that: The temperature sensor is connected to the chip and transmits data to the receiver wirelessly. The gas sensor transmits data to the receiver via wired connection, allowing direct reading of the measured temperature, pressure, and gas concentration data.

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