Reduction reaction device for electrolyte
By designing a level gauge, spray system, and cooling system within the reaction tank during the preparation of vanadium electrolyte, the problems of temperature rise and electrolyte overflow caused by the intense redox reaction were solved, achieving low-cost preparation and safe control of vanadium electrolyte.
Patent Information
- Application Number
- CN202423134804.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-18
- Publication Date
- 2025-12-26
- Estimated Expiration
- 2034-12-18
AI Technical Summary
In the existing vanadium electrolyte preparation process, the redox reaction is violent and difficult to control, which leads to temperature rise, which may cause electrolyte overflow and equipment corrosion. In addition, the existing equipment is costly and has high requirements, making it difficult to achieve low-cost industrialization.
A reduction reaction device including a reaction tank, a level gauge, a spray system, and a cooling system was designed. The level gauge detects the liquid level and activates the spray system and cooling system to control the reaction temperature and liquid level and prevent overflow.
This effectively reduces the reaction temperature, prevents electrolyte overflow, improves the safety and controllability of the device, reduces equipment costs, and enables the low-cost preparation of vanadium electrolyte.
Smart Images
Figure CN223717096U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the field of liquid flow battery, especially a kind of reduction reaction device for electrolyte. BACKGROUND
[0002] Vanadium electrolyte preparation technology mainly has three methods: electrolysis method, chemical reduction method and the method of combination of chemical and electrolysis. Among them, chemical method is difficult to meet the requirements of product quality due to high production cost and difficult to control reaction process, so it is rarely popularized and applied at present. Electrolysis method is difficult to realize industrialization under low cost condition due to high equipment requirement, large power consumption, difficult to control product quality and high equipment investment cost. The method of combination of chemical and electrolysis is currently widely used in vanadium electrolyte production.
[0003] In the reduction stage of the method of combination of chemical and electrolysis, high-purity vanadium pentoxide, high-purity ammonium vanadate and other raw materials are generally added with reducing agent in proper proportion. The reducing agent mainly includes SO2, oxalic acid and the like. When SO2 and other gases are used as reducing agent, the reaction device has high requirements and the reaction process parameters are difficult to control. When oxalic acid is used as reducing agent, it is cheap and green, so it is widely used.
[0004] In the preparation process of vanadium electrolyte, oxidation-reduction reaction occurs and releases heat violently, and the highest temperature can reach about 110 DEG C. At the same time, the reduction system is usually in a strong acid environment. These two factors lead to high requirements for the reduction device. On the other hand, high temperature will make the oxidation-reduction reaction more violent, and the harmful effect is that the oxidation-reduction reaction process is uncontrollable. Violent reaction will produce a lot of carbon dioxide foam, so that the liquid level in the reaction kettle is easy to exceed the alarm, and even the liquid in the reaction kettle will flow out of the reaction kettle with carbon dioxide gas, which will cause great economic loss. UTILITY MODEL CONTENTS
[0005] In view of the above problems of the prior art, the utility model provides a kind of reduction reaction device for electrolyte, can effectively reduce the temperature in reaction device, prevent electrolyte overflow.
[0006] Specifically, the utility model provides a kind of reduction reaction device for electrolyte, including,
[0007] reaction tank body;
[0008] liquid level meter, set up on the reaction tank body, the liquid level meter is used to detect the liquid level of electrolyte in the reaction tank body;
[0009] spraying system, set in the top of the reaction tank body, the spraying system is used to spray spray liquid to the reaction tank body to reduce the liquid level of the electrolyte;
[0010] The cooling system comprises a refrigerating machine, an inlet pipeline and a return pipeline, the refrigerating machine is connected to the reaction tank body through the inlet pipeline and the return pipeline, and the cooling system is used for circulating cooling of electrolyte in the reaction tank body.
[0011] According to one embodiment of the present application, the reduction reaction device further comprises a stirrer arranged at the top of the reaction tank body, and a stirring rod of the stirrer extends downward into the reaction tank body.
[0012] According to one embodiment of the present application, the reduction reaction device further comprises an exhaust pipe arranged at the top of the reaction tank body, and the exhaust pipe is used for exhausting gas and / or acid mist generated in the reaction tank body.
[0013] According to one embodiment of the present application, the liquid level meter comprises a radar liquid level meter and a magnetic flap liquid level meter, the radar liquid level meter is arranged at the top of the reaction tank body, and the magnetic flap liquid level meter is arranged on the side wall of the reaction tank body.
[0014] According to one embodiment of the present application, the reduction reaction device further comprises a temperature sensor arranged on the side wall of the reaction tank body, and the temperature sensor is used for detecting the temperature in the reaction tank body.
[0015] According to one embodiment of the present application, the reaction tank body comprises a shell and an inner lining, and the inner lining is arranged on the inner wall of the shell.
[0016] According to one embodiment of the present application, the material of the shell is carbon steel, and the material of the inner lining is one of PP, PDFE and PVDF.
[0017] According to one embodiment of the present application, the cooling system further comprises a liquid delivery pump arranged on the inlet pipeline.
[0018] According to one embodiment of the present application, the cooling system further comprises an inlet pneumatic valve and an outlet pneumatic valve arranged on the inlet pipeline and the return pipeline respectively.
[0019] According to one embodiment of the present application, a first liquid level and a second liquid level are preset in the reaction tank body, and the second liquid level is higher than the first liquid level.
[0020] If the liquid level of the electrolyte rises to the first liquid level during the reaction process, the liquid level meter triggers the starting of the spraying system.
[0021] If the liquid level of the electrolyte rises to the second liquid level during the reaction process, the liquid level meter triggers the starting of the cooling system.
[0022] The utility model provides a kind of for the reduction reaction device of electrolyte, by setting up spraying system and cooling system to reduce the temperature in reaction device, prevent electrolyte overflow.
[0023] It should be understood that the above general description and the following detailed description of the utility model are exemplary and illustrative, and are intended to provide further explanation of the utility model as claimed. BRIEF DESCRIPTION OF DRAWINGS
[0024] The accompanying drawings are included to provide further explanation of the utility model, they are incorporated and constitute a part of the present application, and the drawings show the embodiment of the utility model, and together with the present specification, it plays the role of explaining the principle of the utility model.The drawings include:
[0025] Figure 1 The perspective view of reduction reaction device of one embodiment of the utility model is shown.
[0026] Among them, the above drawing includes the following reference signs:
[0027] Reduction reaction device 100
[0028] Reaction tank body 110
[0029] Pot shell 1101
[0030] Inner lining 1102
[0031] Solid feeding port 111
[0032] Liquid feeding port 112
[0033] Cooling coil 113
[0034] Liquid outlet pipeline 114
[0035] Pneumatic valve 115
[0036] Liquid level meter 120
[0037] Radar liquid level meter 121
[0038] Magnetic reed liquid level meter 122
[0039] Spraying system 130
[0040] Cooling system 140
[0041] Refrigerator 141
[0042] Liquid inlet pipeline 142
[0043] Return pipeline 143
[0044] Liquid delivery pump 144
[0045] liquid outlet pneumatic valve 145
[0046] liquid outlet pneumatic valve 146
[0047] stirrer 150
[0048] exhaust pipe 160
[0049] temperature sensor 170 DETAILED DESCRIPTION
[0050] It should be noted that the embodiments and features of the embodiments in the present application can be combined with each other without conflict.
[0051] The technical solutions in the embodiments of the present application will be described clearly and completely in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. The description of the at least one exemplary embodiment is actually only illustrative, but not as any limitation on the present application and its application or use. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.
[0052] It should be noted that the terms used herein are only intended to describe specific embodiments, and are not intended to limit the exemplary embodiments according to the present application. As used herein, the singular form is intended to include the plural form, unless the context clearly indicates otherwise, and it should also be understood that when the terms "comprise" and / or "include" are used in the specification, there is a presence of the features, steps, operations, devices, components and / or combinations thereof.
[0053] Unless specifically stated otherwise, the relative arrangements of the components and steps illustrated in these embodiments and the numerical expressions and values set forth herein are not limiting of the scope of the present application. It should be understood that the various parts of the drawings are not necessarily drawn to scale, and that, for the purpose of convenience and clarity, not all components can be shown in a given figure. Techniques, methods, and devices known to those of ordinary skill in the art can not be discussed in detail, but rather can be summarily described in order not to unnecessarily obscure aspects of the present application. In the description of the example embodiments, any specific values should be interpreted as examples only and not as limiting. Other example embodiments of the exemplary embodiments can have different values. It should be noted that like references herein represent like elements or parts throughout the various drawings and that the use of "for example" or "e.g." in connection with a particular item or use of an item does not exclude the use of that item or the use of that item in connection with other items.
[0054] In the description of the present application, it should be understood that the orientation words such as "front, back, up, down, left, right", "transverse, vertical, perpendicular, horizontal" and "top, bottom" and the like indicated orientation or position relationship are generally based on the orientation or position relationship shown in the drawings, only for the convenience of describing the present application and simplifying the description, without making the opposite statement, these orientation words do not indicate and imply that the indicated device or element must have a particular orientation or be constructed and operated in a particular orientation, therefore it cannot be understood as a limitation on the scope of protection of the present application; The orientation words "inner, outer" refer to the inner and outer of the contour of the components themselves.
[0055] In addition, it should be noted that the use of "first", "second" and the like to define parts is only for the convenience of distinguishing the corresponding parts, and the above words have no special meaning unless otherwise stated, therefore it cannot be understood as a limitation on the scope of protection of the present application. In addition, although the terms used in the present application are selected from the commonly known and used terms, some terms mentioned in the specification of the present application may be selected by the applicant according to his or her judgment, and the detailed meaning of each term is explained in the relevant part of the description. In addition, the present application is required to be understood not only by the actual terms used, but also by the meaning implied by each term.
[0056] Figure 1 A perspective view of a reduction reaction device of an embodiment of the present application is shown. As shown in the figure, a reduction reaction device 100 for electrolyte mainly includes a reaction tank body 110, a liquid level meter 120, a spraying system 130 and a cooling system 140.
[0057] Among them, the top of the reaction tank body 110 is usually provided with a solid feeding port 111 and a liquid feeding port 112. The solid feeding port 111 is mainly used to add solid raw materials, such as vanadium-containing raw materials and reducing agents, into the reaction tank body 110. The size of the solid feeding port 111 will be designed according to the particle size and feeding amount of the added solid raw materials. The solid feeding port 111 needs to have a large enough diameter to ensure that the raw materials can smoothly enter the tank body and avoid blockage. The liquid feeding port 112 is used to add various liquid raw materials into the tank body. The liquid raw materials include solvents, reactants or catalysts, etc. In this example, three liquid feeding ports 112 are provided at the top of the reaction tank body 110, which are suitable for adding different liquid reagents into the reaction tank body 110 in a certain proportion to realize a specific chemical reaction.
[0058] The liquid level meter 120 is arranged on the reaction tank body 110. The liquid level meter 120 is used to detect the liquid level of the electrolyte in the reaction tank body 110. The liquid level meter 120 provides real-time liquid level information during the reaction process, and through the real-time liquid level information, the control of the reaction process can be realized to prevent the electrolyte from overflowing.
[0059] The spray system 130 is disposed on the top of the reaction tank body 110. The spray system 130 is used to spray a spray liquid into the reaction tank body 110 to lower the liquid level of the electrolyte. The spray liquid can generally use ultrapure water, which has extremely high purity and contains almost no impurities and ions, and will not interfere with the composition of the electrolyte. During the reaction process, when the liquid level of the electrolyte is too high, it may affect the normal progress of the reaction or bring safety hazards. At this time, the spray system 130 is turned on, which can dilute the electrolyte, lower the temperature in the reaction tank body 110, and play a rapid defoaming role, lower the electrolyte level, and make the reaction process return to normal state.
[0060] The cooling system 140 includes a refrigeration machine 141, a liquid inlet pipeline 142, and a return pipeline 143. The refrigeration machine 141 is connected to the reaction tank body 110 through the liquid inlet pipeline 142 and the return pipeline 143. The cooling system 140 is used to circulate and cool the electrolyte in the reaction tank body 110. The refrigeration machine 141 transfers heat from the electrolyte in the reaction tank body 110 through compression, condensation, expansion, and evaporation processes, thereby achieving cooling in the reaction tank body 110.
[0061] In some examples, the reduction reaction device 100 further includes a stirrer 150. The stirrer 150 is disposed on the top of the reaction tank body 110. The stirring rod of the stirrer 150 extends downward into the reaction tank body 110. The stirrer 150 is used to stir the solid-liquid mixture of the electrolyte in the reaction tank body 110, so that the various components in the mixture are fully mixed, and the heat in the reaction tank body 110 is quickly transferred to avoid local overheating or overcooling. In addition, through stirring, the gas generated in the reaction process can be released from the electrolyte. For example, carbon dioxide and other gases are generated in the rapid reduction reaction of the electrolyte. The stirring of the stirrer 150 enables carbon dioxide to be discharged from the surface of the electrolyte more quickly, preventing the accumulation of gas in the liquid and affecting the normal progress of the reaction.
[0062] In some examples, the reduction reaction device 100 further includes an exhaust pipe 160. The exhaust pipe 160 is disposed on the top of the reaction tank body 110. The exhaust pipe 160 is used to exhaust the gas and / or acid mist generated in the reaction tank body 110. Acid mist is usually a corrosive acid aerosol. If the acid mist remains in the reaction tank body 110, it will cause corrosion to various components inside the tank body, such as the stirrer 150, etc., shortening the service life of these devices. The distal end of the exhaust pipe 160 can be connected to an acid mist absorption tower, which removes the acidic components in the acid mist, thereby avoiding direct discharge of the acid mist into the environment.
[0063] In some examples, the liquid level meter 120 includes a radar liquid level meter 121 and a magnetic float liquid level meter 122. The radar liquid level meter 121 is arranged on the top of the reactor tank body 110, and the magnetic float liquid level meter 122 is arranged on the sidewall of the reactor tank body 110. The radar liquid level meter 121 arranged on the top of the reactor tank body 110 can directly detect the liquid level in the reactor tank body 110 from top to bottom. The radar wave is emitted from the top and vertically downward, and is reflected back when encountering the liquid surface. By measuring the propagation time and other parameters of the radar wave, the height of the liquid level can be accurately calculated. The magnetic float liquid level meter 122 is installed on the sidewall of the reactor tank body 110, which works on the principle of magnetic coupling. The magnetic float in the reactor tank body 110 moves up and down with the change of the liquid level, and drives the flap outside the liquid level meter 120 to flip over through magnetic action, thereby directly displaying the liquid level height. The advantage of installing on the sidewall is that the operator can directly observe the liquid level when inspecting around the tank. The use of two types of liquid level meters 120 improves the accuracy and reliability of liquid level measurement, and enhances the fault tolerance capability. In addition, the intuitive display of the magnetic float liquid level meter 122 allows the operator to quickly understand the general situation of the liquid level in the tank. The radar liquid level meter 121 can record and store the liquid level data, which is beneficial for subsequent reaction control, production analysis and other operations.
[0064] In some examples, the reduction reaction device 100 further includes a temperature sensor 170. The temperature sensor 170 is arranged on the sidewall of the reactor tank body 110, and the temperature sensor 170 is used to detect the temperature in the reactor tank body 110. Multiple temperature sensors 170 can be installed at different positions of the reactor tank body 110 to accurately obtain the temperature distribution data in the reactor tank body 110, which is beneficial for more precise control of the reaction process through temperature data.
[0065] In some examples, the reactor tank body 110 includes a shell 1101 and an inner liner 1102 arranged on the inner wall of the cylindrical shell 1101. Since the electrolyte is usually highly corrosive, the inner liner 1102 needs to be arranged in the shell 1101 to avoid direct corrosion of the shell 1101. The inner liner 1102 can also reduce the wear of the shell 1101. Because there is friction between the solid particles and the inner wall of the tank during the reaction process. That is, the material of the inner liner 1102 usually has good wear resistance, which can avoid the wear of the shell 1101 and maintain the structural integrity of the reactor tank body 110. Preferably, the material of the shell 1101 is carbon steel, and the material of the inner liner 1102 is one of PP, PDFE and PVDF.
[0066] In some examples, the cooling system 140 further comprises a liquid delivery pump 144. The liquid delivery pump 144 is arranged on the liquid inlet pipeline 142. The liquid delivery pump 144 is a power source for circulating the electrolyte in the entire cooling system 140. Under the action of the liquid delivery pump 144, the electrolyte enters the chiller 141 through the liquid inlet pipeline 142, exchanges heat with the cooling liquid, and then returns to the reaction tank body 110 through the return pipeline 143. The liquid delivery pump 144 can adjust the flow of the electrolyte and optimize the heat exchange effect between the electrolytes. When the liquid delivery pump 144 increases the speed, the flow of the electrolyte increases, and the cooling effect is enhanced; on the contrary, when the temperature in the reaction tank body 110 decreases, the speed of the pump can be correspondingly reduced, the flow of the electrolyte is reduced, and the cooling effect is reduced.
[0067] In some examples, the cooling system 140 further comprises a liquid inlet pneumatic valve 145 and a liquid outlet pneumatic valve 146. The liquid inlet pneumatic valve 145 and the liquid outlet pneumatic valve 146 are arranged on the liquid inlet pipeline 142 and the return pipeline 143, respectively. The liquid inlet pneumatic valve 145 and the liquid outlet pneumatic valve 146 can realize the functions of flow regulation and pressure regulation of the circulating pipeline. If integrated with an automatic control system, the adjustment of the valve opening can be realized through a remote control signal, greatly improving the convenience and timeliness of operation.
[0068] In some examples, the first liquid level and the second liquid level are preset in the reaction tank 110, and the second liquid level is higher than the first liquid level. The first liquid level is a safety alarm liquid level, and the second liquid level is an overflow alarm liquid level. If the liquid level of the electrolyte in the reaction tank 110 rises to the first liquid level during the reaction process, the liquid level gauge 120 can trigger the spray system 130 to start working, and continuously spray high-pressure spray liquid into the reaction tank 110 to reduce the liquid level. If the liquid level of the electrolyte continues to rise to the second liquid level during the reaction process, the liquid level gauge 120 can trigger the cooling system 140 to start working. Starting the cooling system 140 to work includes sequentially opening the liquid inlet pneumatic valve 145 and the liquid outlet pneumatic valve 146, starting the liquid delivery pump 144, and starting the power supply of the refrigeration machine 141. The cooling system 140 continuously delivers the electrolyte to the refrigeration machine 141 through the liquid inlet pipeline 142 for heat exchange, and then returns to the reaction tank 110 through the return pipeline 143. As the temperature in the reaction tank 110 decreases, the liquid level of the electrolyte in the reaction tank 110 stabilizes, and when the liquid level decreases to the first liquid level, the refrigeration machine 141 will be immediately turned off, and then the liquid delivery pump 144, the liquid inlet pneumatic valve 145, and the liquid outlet pneumatic valve 146 are turned off. It is easy to understand that, during the entire reaction process, the liquid level in the reaction tank 110 can be controlled below the first liquid level by the spray system 130 and the cooling system 140, that is, the reaction tank 110 is operated in a safe state until the reaction is completed. As an alternative, a first temperature and a second temperature can also be set, and the first temperature and the second temperature correspond to the first liquid level and the second liquid level. Similarly, during the reaction process, when the temperature detected by the temperature sensor 170 reaches the first temperature, the spray system 130 is started to work. When the temperature detected by the temperature sensor 170 continues to rise to the second temperature, the cooling system 140 is started to work. That is, the temperature in the reaction tank 110 obtained by the temperature sensor 170, in combination with the spray system 130 and the cooling system 140, can control the temperature in the reaction tank 110 below the first temperature until the reaction is completed.
[0069] In some examples, the reduction reaction device 100 further comprises a cooling coil 113. The cooling coil 113 is arranged on the inner wall of the reaction tank 110. The cooling coil 113 is connected with a refrigerant for directly reducing the reduction reaction temperature in the reaction tank 110.
[0070] In some examples, the reduction reaction device 100 further comprises a liquid outlet pipeline 114 and a pneumatic valve 115. The liquid outlet pipeline 114 is arranged at the bottom of the reaction tank 110, and the pneumatic valve 115 is arranged on the liquid outlet pipeline 114. By adjusting the opening size of the pneumatic valve 115, the liquid discharge speed in the reaction tank 110 can be controlled according to the needs.
[0071] The following is based on Figure 1 The use process of the reduction reaction device 100 is described as follows:
[0072] Three kinds of liquid raw materials for three different reduction reactions are added through three liquid feeding ports 112 in sequence, the exhaust pipe 160 and the stirrer 150 are started, and the vanadium-containing raw material and the solid reducing agent oxalic acid are added through the solid feeding port 111 in sequence, and the stirrer 150 continuously stirs the mixture of the solid raw material and the liquid raw material;
[0073] With the increase of the reaction time, the heat released in the reduction process increases, which promotes the reduction reaction to be more intense, the carbon dioxide generation speed gradually increases, and the liquid level in the reaction tank body 110 also continuously increases. When the liquid level in the reaction tank body 110 reaches the first liquid level, the spraying system 130 will be opened, and high-pressure spraying liquid will be continuously sprayed into the reaction tank body 110 to reduce the liquid level;
[0074] When the liquid level in the reaction tank body 110 rises to the second liquid level, the cooling system 140 is immediately started. With the decrease of the temperature in the reaction tank body 110, until the liquid level decreases to the first liquid level, the refrigerator 141 will be immediately closed, and then the remaining parts of the cooling system 140 are closed;
[0075] During the reduction reaction, the liquid level in the reaction tank body 110 is controlled below the first liquid level through the spraying system 130 and the cooling system 140 until the reaction is completed.
[0076] It is obvious for those skilled in the art that various modifications and variations can be made to the above exemplary embodiments of the present application without departing from the spirit and scope of the present application. Therefore, it is intended to cover the modifications and variations of the present application falling within the scope of the appended claims and their equivalents.
Claims
1. A device for reduction reaction of electrolyte, characterized by, The application relates to a reaction kettle body, a liquid level meter arranged on the reaction kettle body and used for detecting the liquid level of electrolyte in the reaction kettle body, a spraying system arranged on the top of the reaction kettle body and used for spraying spraying liquid into the reaction kettle body to reduce the liquid level of the electrolyte, a cooling system comprising a refrigerating machine, an inlet pipeline and a return pipeline, the refrigerating machine being connected to the reaction kettle body through the inlet pipeline and the return pipeline, and the cooling system being used for circulating cooling of the electrolyte in the reaction kettle body. The application further comprises a stirrer arranged on the top of the reaction kettle body, and a stirring rod of the stirrer extending downward into the reaction kettle body. The application further comprises an exhaust pipe arranged on the top of the reaction kettle body, and the exhaust pipe being used for exhausting the generated gas and / or acid mist in the reaction kettle body. The liquid level meter comprises a radar liquid level meter arranged on the top of the reaction kettle body and a magnetic flap liquid level meter arranged on the side wall of the reaction kettle body. The application further comprises a temperature sensor arranged on the side wall of the reaction kettle body, and the temperature sensor being used for detecting the temperature in the reaction kettle body.
2. The reduction reaction apparatus according to claim 1, wherein The reaction kettle body comprises a kettle shell and an inner lining arranged on the inner wall of the kettle shell.
3. The reduction reaction apparatus according to claim 1, wherein The material of the kettle shell is carbon steel, and the material of the inner lining is one of PP, PDFE and PVDF.
4. The reduction reaction apparatus according to claim 1, wherein The cooling system further comprises a liquid delivery pump arranged on the inlet pipeline.
5. The reduction reaction apparatus according to claim 1, wherein The cooling system further comprises an inlet pneumatic valve and an outlet pneumatic valve arranged on the inlet pipeline and the return pipeline respectively.
6. The reduction reaction apparatus according to claim 1, wherein The first liquid level and the second liquid level are preset in the reaction kettle body, and the second liquid level is higher than the first liquid level.
7. The reduction reaction apparatus according to claim 6, wherein If the liquid level of the electrolyte rises to the first liquid level during the reaction process, the liquid level meter triggers the spraying system to start.
8. The reduction reaction apparatus according to claim 1, wherein If the liquid level of the electrolyte rises to the second liquid level during the reaction process, the liquid level meter triggers the cooling system to start.
9. The reduction reaction apparatus according to claim 8, wherein 10. The reduction reaction apparatus according to claim 4, wherein