A novel electrolytic cell for hydrogen fluoride electrolysis and a water level measurement method thereof
By using diaphragm group and nitrogen blown tube technology in the hydrogen fluoride electrolytic cell, the gas element concentration of fluorine and hydrogen is reduced, and the liquid level is monitored by measuring strings, the existing electrolytic cell conductors have been solved, and the problems of large contact resistance, cumbersome assembly and maintenance, low output, large energy consumption and high fluorine production cost are achieved, and a more efficient and safe hydrogen fluoride electrolytic process is achieved.
Patent Information
- Application Number
- CN202110282648.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-03-16
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2041-03-16
AI Technical Summary
The existing hydrogen fluoride electrolytic cell has problems such as large conductor contact resistance, cumbersome assembly and maintenance, low output, large energy consumption, and high fluorine production cost, and it is difficult to effectively monitor the liquid level height of the reaction liquid.
A new electrolytic cell was designed, using a diaphragm group to divide the inside of the tank body, and the fluorine and hydrogen gas were replaced by blowing nitrogen tubes to reduce the gas element concentration and enhance safety; the liquid level was monitored by measuring strings to ensure that the electrolyte operated within the stable liquid level range.
It improves the operating efficiency of the electrolytic cell, reduces energy consumption and fluorine production costs, enhances safety, and improves the control ability of reaction materials to ensure that the electrolyte operates in a stable state.
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Figure CN115074755B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a novel electrolytic cell for hydrogen fluoride electrolysis and a water level measurement method thereof. Background Art
[0002] Fluorine is an element with very active chemical properties, and there is almost no free fluorine in nature. The main structure of the current common electrolytic cell types is that the anode and the cathode are separated by an integral diaphragm. The anode is generally connected in such a way that each carbon plate is bolted to a copper hanger or copper frame, and then led out of the cell by a conductive rod. Multiple conductor contact resistances are generated at the connection points between multiple carbon plates and the copper hanger or copper frame, reducing the current efficiency. Multiple carbon plates are connected as a whole, and the workload is large during assembly and maintenance, resulting in low electrolytic cell output, high energy consumption, and high fluorine production cost.
[0003] At the same time, the fluorine and hydrogen produced by the electrolysis of hydrogen fluoride need to be treated in a timely manner to ensure safety. The electrolysis process of hydrogen fluoride is an exothermic state and needs to be cooled in time to avoid affecting the stable electrolysis state of the electrolyte in the electrolytic cell.
[0004] There are also some technical solutions for electrolytic cells for hydrogen fluoride electrolysis in the prior art. For example, a Chinese patent with application number CN201110276871.2 discloses a fluorine gas generating device, including an electrolytic cell, a hydrogen HF remover, a fluorine gas purification pipe, a hydrogen fluoride raw material tank, a hydrogen fluoride liquefier, and a DC power supply, wherein: two heating jackets with a semi-circular cross section are arranged on the electrolytic cell body, and the jackets are provided with a circulating water inlet and a water outlet; the electrolytic cell anode is connected to the anode conductive rod; the anode conductive rod is hollow, and a fluorine gas inlet is opened on the anode conductive rod; the cathode is a cross section of The rectangular ring is adjacent to the outside of the partition between the cathode and anode chambers and is fixed on the top cover by a cathode conductive rod. This technical solution can produce high-purity fluorine gas and meet different use pressures. It has a simple structure, convenient parts replacement and maintenance, a simple operation process, a low price, and can be used anytime. However, this technical solution cannot detect the liquid level of hydrofluoric acid in the electrolytic cell during the reaction. The traditional liquid detection device is easily corroded by hydrofluoric acid. If the liquid level of the reaction liquid is not monitored, the raw material concentration and volume are likely to be insufficient as the reaction proceeds, which is not conducive to the full progress of the reaction.
[0005] In view of this, the present invention proposes a new electrolytic cell for hydrogen fluoride electrolysis and a water level measurement method thereof, which solves the above technical problems. Summary of the invention
[0006] The present invention provides a novel electrolytic cell for hydrogen fluoride electrolysis and a water level measurement method thereof, which can effectively solve the above problems.
[0007] The present invention is achieved in that:
[0008] A novel electrolytic cell for hydrogen fluoride electrolysis described in the present invention comprises a cell body, an anode group, a cathode group, a diaphragm group and a controller; the internal space of the cell body is evenly divided by the diaphragm group, a feeding pipe is also provided on one side of the cell body, and a nitrogen blowing pipe is also provided on the cell body at the top of the feeding pipe; the nitrogen blowing pipe is respectively connected to the inner and outer sides of the diaphragm group in the cell body, and an exhaust pipe is also provided on the outer side of the nitrogen blowing pipe, and the exhaust pipe collects the electrolysis products in the cell body; a cell cover is also provided on the top of the cell body, and an anode conductive rod is also provided on the cell cover, and the bottom of the anode conductive rod is connected to the anode group; the cell cover is placed in a closed state after being installed on the cell body, and the anode group under the cell cover is immersed in the electrolyte outside the diaphragm group in the cell body; the cathode group is installed on the bottom of the cell body inside the diaphragm group; a plurality of measuring strings are also provided on the outer side of the cell body, and the measuring strings are in the shape of vertical chains and are attached to the side wall of the cell body; the measuring strings are used to measure the temperature of different height areas in the cell body, and the controller is used to adjust the operation of the electrolytic cell;
[0009] In the prior art, the fluorine and hydrogen produced by the electrolysis of hydrogen fluoride need to be processed in time to ensure safety. The electrolysis process of hydrogen fluoride is in an exothermic state and needs to be cooled in time to avoid affecting the stable electrolysis state of the electrolyte in the electrolytic cell. In addition, the amount of solution is difficult to control during the reaction. If too much is added, it is easy to affect the overall reaction effect. If there is too little reaction solution in the cell body, the amount of the product after the reaction is likely to be insufficient.
[0010] Therefore, the present invention sets a diaphragm group in the tank body, and during the electrolysis process of hydrogen fluoride, the tank cover is sealed and installed on the tank body, and then the controller is started to control the current parameters transmitted by the conductive rod to the anode group, the hydrogen fluoride in the tank body is electrolyzed, and the fluorine gas and hydrogen generated by the electrolysis are respectively floated and gathered on the inner and outer sides of the diaphragm group, and then the nitrogen introduced through the nitrogen blowing pipe makes the fluorine gas and hydrogen in the tank body be collected through the exhaust pipe along with the circulating nitrogen, and then the hydrogen fluoride is dissolved in a set aqueous solution, and the hydrogen fluoride is supplemented from the bottom of the tank body through the one-way valve in the feeding pipe, and the hydrogen fluoride is measured by the series The amount of hydrogen fluoride aqueous solution in the cell body is obtained, so that the hydrogen fluoride in the cell body is in a state of submerging the diaphragm group, ensuring that the electrolysis process of hydrogen fluoride is in a stable liquid level range in the cell body; the present invention utilizes the arranged diaphragm group to evenly divide the inside of the cell body, replaces the prepared fluorine gas and hydrogen gas through a nitrogen blowing pipe, reduces the concentration of its gas element and enhances safety, adopts a measuring string to monitor the liquid level of hydrofluoric acid from outside the cell body, improves the control of the reaction materials during the reaction, and then makes the electrolyte in a stable electrolysis state, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0011] Preferably, the cell cover is further provided with a sealing box, which is made of insulating material and is sleeved on the anode conductive rod; the sealing box is used to maintain the anode conductive rod in a sealed state on the cell cover; during operation, after the cell cover is installed on the cell body, the position of the anode group needs to be controlled by the anode conductive rod, and the cell cover often uses calcium fluoride sealing materials, which are inconvenient to install and are prone to leakage under the influence of hydrogen fluoride electrolyte; therefore, the present invention sleeves the sealing box on the anode conductive rod through the provided sealing box, and then after adjusting the position of the anode group under the cell cover, the sealing box is used to finally seal the anode conductive rod on the cell cover, thereby ensuring the sealing performance of the cell cover after being installed on the cell body, thereby maintaining the operating effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0012] Preferably, the measuring string is provided with several groups and is closely attached to the side wall of the tank body at the same height, the measuring string includes thermoelectric plates distributed along the longitudinal direction of the tank body, the thermoelectric plates are electrically connected together by conduction lines, and the thermoelectric plates are communicated with the controller through the conduction lines; as the reaction proceeds, the liquid level in the tank body continuously decreases, and during the reaction, there is a significant difference between the temperature in the solution and the temperature of the air above the liquid surface, the height of the liquid surface can be obtained by measuring the temperature between the two reaction zones by the thermoelectric plates, the monitoring instrument in the reaction does not need to directly contact the solution, and the installation cost is low, and it can also ensure that the temperature of the electrolyte is within a stable range, thereby maintaining the operating effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0013] Preferably, the anode group further includes a carbon plate, a copper hanger and a carbon fiber splint; the surface of the carbon plate is nickel-plated; the top of the copper hanger is connected to the anode conductive rod on the tank cover, and a carbon fiber splint is installed on the bottom of the copper hanger, and the copper hanger fixes the carbon plate through the carbon fiber splint; during operation, since the hydrogen fluoride material in the electrolyte is strongly acidic, it will corrode the carbon plate in the anode group after repeated use, weakening the electrolytic performance of the carbon plate, and the copper splint is easily deformed under the reaction force when clamping the carbon plate, and will also cause corrosion and contaminate the electrolytic cell during immersion in the hydrogen fluoride electrolyte; therefore The present invention enhances the strength, conductivity and corrosion resistance of the carbon plate by nickel-plating the surface of the carbon plate, greatly prolonging the service life of the carbon plate, and can adjust the carbon plate to an optimal spacing position with the diaphragm group by connecting the copper hanger to the anode conductive rod on the tank cover, and replaces the copper splint with the carbon fiber splint to solve the problem of low strength and corrosion of the copper splint. At the same time, the toughness of the carbon fiber splint avoids damage to the nickel-plated layer when rigidly connected to the carbon plate, ensuring the stable state of the anode group during the electrolysis process, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0014] Preferably, the cathode group further comprises a cathode frame and a cathode plate; the cathode frame is installed inside the diaphragm group in the tank body, the cathode frame is connected by a telescopic rod in a plane direction perpendicular to the diaphragm group, and a cathode cavity is left at the top of the cathode frame in the diaphragm group; the cathode plate is installed in the cathode frame by a damping shaft and adjusted to an inclined state; during operation, fluorine gas and hydrogen gas generated by hydrogen fluoride will float up in the electrolyte solution, and if the two are mixed in the electrolyte solution, the purity of the product collected by the exhaust pipe will be destroyed, and a safety hazard will also occur; therefore, the present invention arranges the cathode frame at The interior of the diaphragm group is provided with a cathode cavity, so that the electrolysis products are collected by exhaust pipes on both sides of the diaphragm group, respectively, so that the hydrogen generated by the cathode can completely enter the cathode cavity without escaping from the diaphragm group, thereby ensuring the safety of operation. The cathode plate installed in the cathode frame through the damping shaft can adjust the deflection state of the cathode plate according to the set electrolysis rate, and cooperate with the telescopic rod installed in the cathode frame to adjust the distance between the cathode plate and the diaphragm group, so that the hydrogen generated on the cathode plate can be smoothly discharged into the cathode cavity, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0015] Preferably, the diaphragm group is an inverted U-shaped structure, and a fixed small cover plate is further arranged above the diaphragm group; a large cover plate is further arranged on the outer side of the small cover plate, and the small cover plate is snap-fitted and installed in the large cover plate, and the small cover plate and the large cover plate are matched with the size of the diaphragm group and the cell body respectively; during operation, the diaphragm group in the electrolytic cell will produce loss in the electrolyte environment after long-term operation, and the disassembly of the diaphragm group in the prior art requires the corresponding disassembly of the large cover plate and the cathode group components in the electrolytic cell before the diaphragm group can be taken out, which is not convenient for the diaphragm group. The membrane group is inspected and repaired; the small cover plate is arranged in the present invention to make it integrated with the diaphragm group, and then when the diaphragm group is inspected and repaired, it is only necessary to move the tank cover and directly take out the small cover plate in the large cover plate, so that the diaphragm group can be taken out from the tank body, avoiding the operation of removing the large cover plate and the cathode group, and by optimizing the size of the diaphragm group in the tank body, ensuring the distance between the carbon plate and the diaphragm, the fluorine gas generated on the anode does not penetrate into the diaphragm group, ensuring the safety of operation, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0016] The present invention also includes a water level measurement method, which is divided into the following steps:
[0017] S1, evenly distribute the thermoelectric sheets for measurement along the outer wall of the measured container, and the thermoelectric sheets are connected together by conductive wires,
[0018] S2, the measured container begins to react. During the reaction, the temperature of the solution in the container rises, and as the reaction proceeds, part of the solution is reacted into gas, and the liquid level of the solution continues to drop.
[0019] S3, the temperature of the side wall in contact with the solution in the container is higher, and the temperature of this point is measured by the thermoelectric sheet in the lower part as T1, while the temperature of the side wall not in contact with the solution is lower, and the temperature of this point is measured by the thermoelectric sheet in the upper part as T2. It can be obtained that T1>T2,
[0020] S4, define the lower thermoelectric sheet as A, and the upper thermoelectric sheet as B. When A and B have the maximum temperature difference, that is, T1-T2 is the maximum value, it can be obtained that the range between A and B at this time is between the liquid and above the liquid surface. The range of the liquid level can be determined by determining which two thermoelectric sheets have the largest temperature difference.
[0021] Preferably, a thermoelectric sheet is defined as C, and C is a warning point. When C is equal to B, it means that the solution has dropped below the warning point, and C sends an alarm signal to the controller.
[0022] The beneficial effects of the present invention are as follows:
[0023] 1. The present invention replaces the prepared fluorine gas and hydrogen gas through a nitrogen blowing pipe, thereby reducing the concentration of the gas element and enhancing safety. The sealing box is used to perform the final sealing on the anode conductive rod on the tank cover to ensure the sealing performance of the tank cover after being installed on the tank body.
[0024] 2. The present invention can monitor the temperature at each point by setting thermoelectric plates on the measuring string, which are evenly distributed on the outer wall of the entire tank body, and can determine the height of the solution in the tank body according to the temperature difference between the solution and the air above the solution. When the solution in the tank body drops to the warning water level, an alarm can be issued to prompt the staff to add materials in time to ensure the stable progress of the reaction and the normal synthesis of the product.
[0025] 3. The present invention arranges the cathode frame inside the diaphragm group so that the electrolysis products are collected by the exhaust pipes on both sides of the diaphragm group, so that the hydrogen generated by the cathode can completely enter the cathode cavity, ensuring the safety of operation; the small cover plate is arranged as a whole with the diaphragm group, thereby avoiding the operation of removing the large cover plate and the cathode group when repairing the diaphragm group. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.
[0027] The present invention is further described below in conjunction with the accompanying drawings and implementation modes.
[0028] Figure 1 is a three-dimensional diagram of an electrolytic cell in the present invention;
[0029] Figure 2 is an exploded view of the electrolytic cell components of the present invention;
[0030] Figure 3 is a cross-sectional view of an electrolytic cell component of the present invention;
[0031] Figure 4 yes Figure 2 A partial enlarged view of the middle A;
[0032] Figure 5 yes Figure 3 A partial enlarged view of point B in the middle;
[0033] In the figure: tank 1, measuring string 11, feeding pipe 12, nitrogen blowing pipe 13, exhaust pipe 14,
[0034] Thermoelectric sheet 111, conductive wire 112,
[0035] Anode group 2, carbon plate 21, copper hanger 22, carbon fiber splint 23,
[0036] Cathode group 3, cathode frame 31, telescopic rod 311, cathode plate 32, damping shaft 321,
[0037] Diaphragm group 4, small cover plate 41, large cover plate 42,
[0038] Tank cover 5, anode conductive rod 51, sealing box 52. DETAILED DESCRIPTION
[0039] In order to make the embodiments of the present invention, all belong to the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents the selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work belong to the scope of protection of the present invention.
[0040] In the description of the present invention, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as referring to the purpose, technical solutions and advantages of the methods. To be more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work indicate or imply relative importance or implicitly indicate the number of indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "multiple" is two or more, unless otherwise clearly and specifically defined.
[0041] like Figures 1 to 5 As shown, a novel electrolytic cell for hydrogen fluoride electrolysis described in the present invention comprises a cell body 1, an anode group 2, a cathode group 3, a diaphragm group 4 and a controller; the internal space of the cell body 1 is evenly divided by the diaphragm group 4, a feeding pipe 12 is further provided on one side of the cell body 1, and a nitrogen blowing pipe 13 is further provided on the cell body 1 at the top of the feeding pipe 12; the nitrogen blowing pipe 13 is respectively connected to the inner and outer sides of the diaphragm group 4 in the cell body 1, and an exhaust pipe 14 is further provided on the outer side of the nitrogen blowing pipe 13, and the exhaust pipe 14 collects the electrolysis products in the cell body 1; a cell cover 5 is further provided on the top of the cell body 1, and the cell cover 5 is also provided with an anode conductive rod 51, the bottom of the anode conductive rod 51 is connected to the anode group 2; the tank cover 5 is installed to the tank body 1 so that it is in a closed state, and the anode group 2 under the tank cover 5 is immersed in the electrolyte outside the diaphragm group 4 in the tank body 1; the cathode group 3 is installed on the bottom of the tank body 1 inside the diaphragm group 4; the outer side of the tank body 1 is also provided with a plurality of measuring strings 11, the measuring strings 11 are vertical chain-shaped and attached to the side wall of the tank body 1; the measuring strings 11 are used to measure the temperature of different height areas in the tank body 1, and the controller is used to adjust the operation of the electrolytic cell;
[0042] In the prior art, the fluorine gas and hydrogen gas produced by the electrolysis of hydrogen fluoride need to be processed in time to ensure safety, and the electrolysis process of hydrogen fluoride is in an exothermic state, and needs to be cooled in time to avoid affecting the stable electrolysis state of the electrolyte in the electrolytic cell. In addition, the amount of the solution is difficult to control during the reaction. If too much is added, it is easy to affect the overall reaction effect. If there is too little reaction solution in the tank body 1, it is easy to have insufficient amount of the product after the reaction.
[0043] Therefore, the present invention sets a diaphragm group 4 in the tank body 1, and during the electrolysis of hydrogen fluoride, the tank cover 5 is sealed and installed on the tank body 1, and then the controller is started to control the current parameters transmitted by the conductive rod to the anode group 2, the hydrogen fluoride in the tank body 1 is electrolyzed, and the fluorine gas and hydrogen generated by the electrolysis are respectively floated and gathered on the inner and outer sides of the diaphragm group 4, and then the nitrogen introduced through the nitrogen blowing pipe 13 is used to collect the fluorine gas and hydrogen in the tank body 21 along with the circulating nitrogen through the exhaust pipe 14, and then the hydrogen fluoride is dissolved in a set aqueous solution, and the hydrogen fluoride is supplemented from the bottom of the tank body 1 through the one-way valve in the feeding pipe 12, and the hydrogen fluoride is measured. The measuring string 11 obtains the amount of hydrogen fluoride aqueous solution in the cell body 1, so that the hydrogen fluoride in the cell body 1 is in a state of submerging the diaphragm group 4, ensuring that the electrolysis process of hydrogen fluoride is in a stable liquid level range in the cell body 1; the present invention utilizes the arranged diaphragm group 4 to evenly separate the inside of the cell body 1, replaces the prepared fluorine gas and hydrogen gas through the nitrogen blowing tube 13, reduces the concentration of the gas element and enhances the safety, and uses the measuring string 11 to monitor the liquid level of hydrofluoric acid from outside the cell body 1, thereby improving the control of the reaction materials during the reaction process, and then makes the electrolyte in a stable electrolysis state, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0044] As an embodiment of the present invention, a sealing box 52 is further provided on the tank cover 5, and the sealing box 52 is made of insulating material and is sleeved on the anode conductive rod 51; the sealing box 52 is used to maintain the sealed state of the anode conductive rod 51 on the tank cover 5; during operation, after the tank cover 5 is installed on the tank body 1, the position of the anode group 2 needs to be controlled by the anode conductive rod 51, and the tank cover 5 often uses calcium fluoride sealing materials, which is inconvenient to install and is prone to leakage under the influence of hydrogen fluoride electrolyte; therefore, the present invention sets a sealing box 52, sleeves it on the anode conductive rod 51, and then after adjusting the position of the anode group 2 below the tank cover 5, the sealing box 52 is used to finally seal the anode conductive rod 51 on the tank cover 5, thereby ensuring the sealing performance of the tank cover 5 after being installed on the tank body 1, thereby maintaining the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0045] As an embodiment of the present invention, the measuring string 11 is provided with several groups and is closely attached to the side wall of the tank body 1 at the same height. The measuring string 11 includes thermoelectric plates 111 distributed along the longitudinal direction of the tank body 1. The thermoelectric plates 111 are electrically connected together through conductive lines 112, and the thermoelectric plates 111 are communicated with the controller through conductive lines 112. As the reaction proceeds, the liquid level in the tank body 1 continuously decreases, and during the reaction, the temperature in the solution and the temperature of the air above the liquid surface are significantly different. The height of the liquid surface can be obtained by measuring the temperature between the two reaction zones through the thermoelectric plates 111. The monitoring instrument in the reaction does not need to directly contact the solution, and the installation cost is low. It can also ensure that the temperature of the electrolyte is within a stable range, thereby maintaining the operating effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0046] As an embodiment of the present invention, the anode group 2 also includes a carbon plate 21, a copper hanger 22 and a carbon fiber splint 23; the surface of the carbon plate 21 is nickel-plated; the top of the copper hanger 22 is connected to the anode conductive rod 51 on the tank cover 5, and the carbon fiber splint 23 is installed on the bottom of the copper hanger 22, and the copper hanger 22 fixes the carbon plate 21 through the carbon fiber splint 23; during operation, since the hydrogen fluoride material in the electrolyte is strongly acidic, it will corrode the carbon plate 21 in the anode group 2 after repeated use, weakening the electrolytic performance of the carbon plate 21, and at the same time, the copper splint is easily deformed under the reaction force when clamping the carbon plate 21, and corrosion will also occur during the immersion in the hydrogen fluoride electrolyte. and contaminate the electrolytic cell; therefore, the present invention enhances the strength, conductivity and corrosion resistance of the carbon plate 21 by nickel-plating the surface of the carbon plate 21, greatly prolongs the service life of the carbon plate 21, and by connecting the copper hanger 22 to the anode conductive rod 51 on the tank cover 5, the carbon plate 21 can be adjusted to an optimal spacing position with the diaphragm group 4, and the copper splint is replaced by the carbon fiber splint 23, which solves the problem of low strength and corrosion of the copper splint. At the same time, the toughness of the carbon fiber splint 23 avoids damage to the nickel plating layer when it is rigidly connected to the carbon plate 21, thereby ensuring the stability of the anode group 2 during the electrolysis process, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0047] As an embodiment of the present invention, the cathode group 3 also includes a cathode frame 31 and a cathode plate 32; the cathode frame 31 is installed inside the diaphragm group 4 in the tank body 1, and the cathode frame 31 is connected by a telescopic rod 311 in a plane direction perpendicular to the diaphragm group 4, and a cathode cavity is left at the top of the cathode frame 31 in the diaphragm group 4; the cathode plate 32 is installed in the cathode frame 31 through a damping shaft 321 and adjusted to an inclined state; during operation, the fluorine gas and hydrogen generated by hydrogen fluoride will float up in the electrolyte solution, and if the two are mixed in the electrolyte solution, it will not only destroy the purity of the product collected by the exhaust pipe 14, but also cause safety hazards; therefore, the present invention is achieved by The pole frame 31 is arranged inside the diaphragm group 4, and a cathode cavity is formed inside the diaphragm group 4, so that the electrolysis products are collected by the exhaust pipes 14 on the inner and outer sides of the diaphragm group 4 respectively, so that the hydrogen generated by the cathode can completely enter the cathode cavity without escaping from the diaphragm group 4, thereby ensuring the safety of operation. The cathode plate 32 installed in the cathode frame 31 through the damping shaft 321 can adjust the deflection state of the cathode plate 32 according to the set electrolysis rate, and cooperate with the telescopic rod 311 installed in the cathode frame 31 to adjust the distance between the cathode plate 32 and the diaphragm group 4, so that the hydrogen generated on the cathode plate 32 can be smoothly discharged into the cathode cavity, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0048] As an embodiment of the present invention, the diaphragm group 4 is an inverted U-shaped structure, and a fixed small cover plate 41 is further provided above the diaphragm group 4; a large cover plate 42 is further provided on the outer side of the small cover plate 41, and the small cover plate 41 is snap-fitted and installed in the large cover plate 42, and the small cover plate 41 and the large cover plate 42 are respectively matched with the size of the diaphragm group 4 and the cell body 1; during operation, the diaphragm group 4 in the electrolytic cell will produce loss in the electrolyte environment after long-term operation, and the disassembly of the diaphragm group 4 in the prior art requires the corresponding disassembly of the large cover plate 42 and the cathode group 3 components in the electrolytic cell before the diaphragm group 4 can be removed. 4, it is inconvenient to inspect and repair the diaphragm group 4; the present invention integrates the small cover plate 41 with the diaphragm group 4, and then when inspecting the diaphragm group 4, it is only necessary to move the tank cover 5 and directly take out the small cover plate 41 in the large cover plate 42, so that the diaphragm group 4 can be taken out from the tank body 1, avoiding the operation of removing the large cover plate 42 and the cathode group 3, and by optimizing the size of the diaphragm group 4 in the tank body 1, ensuring the distance between the carbon plate 21 and the diaphragm, the fluorine gas generated on the anode does not penetrate into the diaphragm group 4, ensuring the safety of operation, thereby improving the operation effect of the new electrolytic cell for hydrogen fluoride electrolysis.
[0049] The present invention also includes a water level measurement method, which is divided into the following steps:
[0050] S1, the thermoelectric sheets 111 for measurement are evenly distributed along the outer wall of the measured container, and the thermoelectric sheets 111 are connected together through the conductive wires 112,
[0051] S2, the measured container begins to react. During the reaction, the temperature of the solution in the container rises, and as the reaction proceeds, part of the solution is reacted into gas, and the liquid level of the solution continues to drop.
[0052] S3, the temperature of the side wall of the container in contact with the solution is higher, and the temperature of this point is measured by the thermoelectric sheet 111 in the lower part as T1, while the temperature of the side wall of the part not in contact with the solution is lower, and the temperature of this point is measured by the thermoelectric sheet 111 in the upper part as T2, so T1>T2,
[0053] S4, define the lower thermoelectric plate 111 as A, and the upper thermoelectric plate 111 as B. When A and B have the maximum temperature difference, that is, T1-T2 is the maximum value, the range between A and B at this time is between the liquid and above the liquid surface. The range of the liquid level can be determined by determining which two thermoelectric plates 111 have the largest temperature difference.
[0054] It should be particularly emphasized here that the water level measurement method can be used not only in the electrolytic cell of the present invention, but also in the electrolytic cell of any exothermic reaction or endothermic reaction. As long as there is a temperature change during the reaction, the liquid level during the reaction can be determined.
[0055] As an embodiment of the present invention, a thermoelectric plate 111 is defined as C, and C is a warning point. When C is B, it means that the solution has dropped below the warning point. C sends an alarm signal to the controller. After the liquid level drops to the warning point, the controller automatically sends an alarm signal. There is no need for manual monitoring and timed reaction time, so the quality of the reactants can be better controlled.
[0056] During operation, by setting the diaphragm group 4 in the tank body 1, during the electrolysis of hydrogen fluoride, the tank cover 5 is sealed and installed on the tank body 1, and then the controller is started to control the current parameters transmitted by the conductive rod to the anode group 2, the hydrogen fluoride in the tank body 1 is electrolyzed, and the fluorine gas and hydrogen gas generated by the electrolysis are respectively floated and gathered on the inner and outer sides of the diaphragm group 4, and then the nitrogen gas introduced through the nitrogen blowing pipe 13 is used to make the fluorine gas and hydrogen gas inside the tank body 21 be collected through the exhaust pipe 14 along with the circulating nitrogen gas, and then the hydrogen fluoride is dissolved in the set aqueous solution, and the hydrogen fluoride is supplemented from the bottom of the tank body 1 through the one-way valve in the feeding pipe 12, and the amount of hydrogen fluoride aqueous solution in the tank body 1 is obtained through the measuring string 11 , so that the hydrogen fluoride in the tank body 1 is in a state of submerging the diaphragm group 4, ensuring that the electrolysis process of hydrogen fluoride is in a stable liquid level range in the tank body 1; the sealing box 52 is set, which is sleeved on the anode conductive rod 51, and then after adjusting the position of the anode group 2 under the tank cover 5, the sealing box 52 is used to finally seal the anode conductive rod 51 on the tank cover 5 to ensure the sealing performance of the tank cover 5 after it is installed on the tank body 1; the thermoelectric plate 111 set on the measuring string 11 is evenly distributed on the outer side wall of the entire tank body, and can monitor the temperature at each point, and can determine the height of the solution in the tank body according to the temperature difference between the solution and the air above the solution, and can When the solution in the tank body drops to the warning water level, an alarm is issued to prompt the staff to add materials in time to ensure the stable progress of the reaction and the normal synthesis of the product; the surface of the carbon plate 21 is nickel-plated to enhance the strength, conductivity and corrosion resistance of the carbon plate 21, greatly extending the service life of the carbon plate 21, and by connecting the copper hanger 22 to the anode conductive rod 51 on the tank cover 5, the carbon plate 21 can be adjusted to the optimal spacing position with the diaphragm group 4, and the carbon fiber splint 23 is used to replace the copper splint, which solves the problem of low strength and corrosion of the copper splint. At the same time, the toughness of the carbon fiber splint 23 avoids damage to the nickel plating layer when it is rigidly connected to the carbon plate 21. The cathode frame 31 is arranged inside the diaphragm group 4, and a cathode cavity is formed inside the diaphragm group 4, so that the electrolysis products are collected by the exhaust pipes 14 on both sides of the diaphragm group 4, so that the hydrogen generated by the cathode can completely enter the cathode cavity without escaping from the diaphragm group 4, ensuring the safety of operation, and the cathode plate 32 installed in the cathode frame 31 through the damping shaft 321 can adjust the deflection state of the cathode plate 32 according to the set electrolysis rate, and cooperate with the telescopic rod 311 installed in the cathode frame 31 to adjust the distance between the cathode plate 32 and the diaphragm group 4, so that the hydrogen generated on the cathode plate 32 can be smoothly discharged into the cathode cavity;The small cover plate 41 is provided so as to be integrated with the diaphragm group 4. When the diaphragm group 4 is inspected, it is only necessary to remove the tank cover 5 and directly take out the small cover plate 41 in the large cover plate 42 to remove the diaphragm group 4 from the tank body 1, thereby avoiding the operation of removing the large cover plate 42 and the cathode group 3. By optimizing the size of the diaphragm group 4 in the tank body 1, the distance between the carbon plate 21 and the diaphragm is ensured, so that the fluorine gas generated on the anode does not enter the diaphragm group 4, thereby ensuring the safety of operation. ;
[0057] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. A method for measuring the water level of an electrolytic cell for hydrogen fluoride electrolysis, characterized in that: It comprises a tank body (1), an anode group (2), a cathode group (3), a diaphragm group (4) and a controller. The internal space of the cell body (1) is evenly divided by the diaphragm group (4); a feeding pipe (12) is also provided on one side of the cell body (1); a nitrogen blowing pipe (13) is also provided on the cell body (1) at the top of the feeding pipe (12); the nitrogen blowing pipe (13) is respectively connected to the inner and outer sides of the diaphragm group (4) in the cell body (1); an exhaust pipe (14) is also provided on the outer side of the nitrogen blowing pipe (13); the exhaust pipe (14) collects the electrolysis products in the cell body (1); The top of the cell body (1) is also provided with a cell cover (5), and the cell cover (5) is also provided with an anode conductive rod (51), and the bottom of the anode conductive rod (51) is connected to the anode group (2); after the cell cover (5) is installed on the cell body (1), it is in a sealed state, and the anode group (2) below the cell cover (5) is immersed in the electrolyte outside the diaphragm group (4) in the cell body (1); the cathode group (3) is installed on the bottom of the cell body (1) inside the diaphragm group (4); the outer side of the cell body (1) is also provided with a plurality of measuring strings (11), and the measuring strings (11) are in the shape of vertical chains and are attached to the side wall of the cell body (1); the measuring strings (11) are used to measure the temperature of different height areas in the cell body (1), and the controller is used to adjust the operation of the electrolytic cell; the cathode group (3) also includes a cathode frame (31) and a cathode plate (32 ); the cathode frame (31) is installed inside the diaphragm group (4) in the cell body (1); the cathode frame (31) is connected in a plane direction perpendicular to the diaphragm group (4) by a telescopic rod (311); and a cathode cavity is left at the top of the cathode frame (31) inside the diaphragm group (4); the cathode plate (32) is installed in the cathode frame (31) by a damping shaft (321) and adjusted to an inclined state; the cathode plate (32) installed in the cathode frame (31) by the damping shaft (321) can adjust the deflection state of the cathode plate (32) according to a set electrolysis rate, and cooperate with the telescopic rod (311) installed in the cathode frame (31) to adjust the distance between the cathode plate (32) and the diaphragm group (4), so that the hydrogen generated on the cathode plate (32) is smoothly discharged into the cathode cavity, thereby improving the operation effect of the electrolytic cell for hydrogen fluoride electrolysis; The method comprises the following steps: S1, evenly distributing thermoelectric sheets (111) for measurement along the outer wall of the container to be measured, wherein the thermoelectric sheets (111) are connected together via conductive lines (112), S2, the measured container begins to react. During the reaction, the temperature of the solution in the container rises, and as the reaction proceeds, part of the solution is reacted into gas, and the liquid level of the solution continues to drop. S3, the temperature of the side wall of the container in contact with the solution is higher, and the temperature of this point is measured by the thermoelectric sheet (111) in the lower part as T1, while the temperature of the side wall of the container not in contact with the solution is lower, and the temperature of this point is measured by the thermoelectric sheet (111) in the upper part as T2. It can be obtained that T1>T2, S4, define the lower thermoelectric sheet (111) as A, and the upper thermoelectric sheet (111) as B. When A and B have the maximum temperature difference, that is, T1-T2 is the maximum value, it can be obtained that the range between A and B at this time is between the liquid and above the liquid surface. By determining which two thermoelectric sheets (111) have the largest temperature difference, the range of the liquid level can be determined.
2. The water level measurement method according to claim 1, characterized in that: The tank cover (5) is also provided with a sealing box (52), which is made of insulating material and is sleeved on the anode conductive rod (51); the sealing box (52) is used to maintain the anode conductive rod (51) in a sealed state on the tank cover (5).
3. The water level measurement method according to claim 1, characterized in that: The measuring string (11) is provided with a plurality of groups and is closely attached to the side wall of the tank body (1) at the same height. The measuring string (11) comprises thermoelectric sheets (111) distributed along the longitudinal direction of the tank body (1). The thermoelectric sheets (111) are electrically connected together via conduction lines (112). The thermoelectric sheets (111) are in communication with the controller via the conduction lines (112).
4. The water level measurement method according to claim 1, characterized in that: The anode group (2) further comprises a carbon plate (21), a copper hanger (22) and a carbon fiber splint (23); the surface of the carbon plate (21) is nickel-plated; the top end of the copper hanger (22) is connected to the anode conductive rod (51) on the tank cover (5), and the carbon fiber splint (23) is installed on the bottom end of the copper hanger (22); the copper hanger (22) fixes the carbon plate (21) via the carbon fiber splint (23).
5. The water level measurement method according to claim 1, characterized in that: The diaphragm group (4) is an inverted U-shaped structure, and a fixed small cover plate (41) is also arranged above the diaphragm group (4); a large cover plate (42) is also arranged on the outer side of the small cover plate (41), and the small cover plate (41) is snap-fitted and installed in the large cover plate (42), and the small cover plate (41) and the large cover plate (42) respectively match the sizes of the diaphragm group (4) and the tank body (1).
6. The water level measurement method according to claim 1, characterized in that: A thermoelectric sheet (111) is defined as C, and C is a warning point. When C is equal to B, it means that the solution has dropped below the warning point, and C sends an alarm signal to the controller.
Citation Information
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