CN216799833U - Continuous reactor for synthesizing high-crystallinity nanoscale solid electrolyte precursor - Google Patents
Continuous reactor for synthesizing high-crystallinity nanoscale solid electrolyte precursor Download PDFInfo
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Abstract
The utility model relates to a continuous reactor for synthesizing a high-crystallinity nanoscale solid electrolyte precursor, which comprises a reaction kettle body, and a stirring device, a heating device and a feeding controller which are arranged on the reaction kettle body; the reaction kettle also comprises a temperature sensor, wherein the temperature sensor is arranged in the reaction kettle body and used for monitoring the reaction temperature and transmitting a temperature signal to the heating device, and the heating device is opened and closed according to the temperature signal; still include the pH sensor, the pH sensor sets up inside the reation kettle body, and the pH sensor is used for monitoring reaction pH value to with pH value signal transmission extremely feeding controller, feeding controller adds acid-base regulator according to pH value signal. The continuous reactor can monitor the temperature and the pH value of a reaction system in real time, transmit signals to the heating device and the feeding controller, and automatically and accurately adjust the temperature and the pH value in the reaction process, so that the reaction is smoothly carried out.
Description
Technical Field
The utility model belongs to the field of solid electrolytes, and particularly relates to a continuous reactor for synthesizing a high-crystallinity nanoscale solid electrolyte precursor.
Background
Most of lithium ion secondary batteries in the current market adopt liquid electrolytes, so that the production process is limited to a great extent, the moisture control is very strict on the environmental requirement of assembly, and the liquid electrolytes have the safety problems of package leakage, current collector corrosion, over-high temperature explosion and the like in the application of subsequent products. In addition, the liquid electrolyte generally has a phenomenon of cycle capacity fading due to the problems of protective film (SEI) generation, gas generation by side reactions, decomposition at high temperature and high pressure, and the like in electrochemical reactions. If the solid electrolyte is adopted, the problems can be effectively improved, the solid electrolyte has the characteristics of high safety and long service life, the electrolyte is replaced in assembly, the diaphragm is also used, the structure of the battery is greatly simplified, the design with higher energy density can be achieved, the design is more flexible and convenient in profile design, the requirements on equipment and environment are reduced in production due to no need of air isolation, and most of fixed asset cost is saved.
Solid-state battery materials currently fall into two main categories: the first type is polymer type (gel type) electrolyte, including polyether (polyethylene oxide, PEO), Polyacrylonitrile (PAN), Polymethacrylate (PMMA), polyvinylidene fluoride (PVDF), etc., although the polymer electrolyte can obviously overcome some disadvantages of liquid lithium ion batteries in development and application, there are still some problems to be solved: for example, the ionic conductivity is low at normal temperature, the compatibility with electrodes is poor, and the mechanical strength is still insufficient. The second type is inorganic solid electrolyte, which has higher thermodynamic stability and mechanical strength, can be charged and discharged with large current, and can be used in large currentThe full performance is high. The inorganic type solid electrolyte is further classified into a crystalline electrolyte and an amorphous electrolyte according to its crystal structure. The main research currently developed for crystalline electrolytes is perovskite (ABO)3) Type structure, lithium ion electrolyte, NASICON type structure lithium ion electrolyte, LISICON type structure lithium ion electrolyte, etc. The synthesis of NASICON type structure lithium ion electrolyte is especially important, and the chemical formula of NASICON is AB2(PO4)3(A is a monovalent metal element such as Li, Na, K, Rb or Cs, etc., and B is a tetravalent element such as Ti, Zr, Ge, Si or Sn).
At present, the NASICON synthesis mode mostly adopts a hydrothermal reduction method, a solid-state sintering method and a sol-gel method. The batch quantity of the hydrothermal reduction method is too small, and the method is not suitable for industrial mass production; the material obtained by the solid state sintering method has larger grain diameter and poor uniformity, and is difficult to match with electrode materials when a battery is assembled, because the stoichiometry and the heating temperature are difficult to control; the sol-gel method has the disadvantages of long production time, severe requirements on the pH value control and the temperature control of a system, and difficulty in meeting the requirements of the existing equipment.
Therefore, the technical scheme of the utility model is provided.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems in the prior art, the utility model provides a continuous reactor for synthesizing a high-crystallinity nano-scale solid electrolyte precursor. The continuous reactor can monitor the temperature and the pH value of a reaction system in real time, transmit signals to the heating device and the feeding controller, and automatically and accurately adjust the temperature and the pH value in the reaction process, so that the reaction is smoothly carried out.
The utility model provides a continuous reactor for synthesizing a high-crystallinity nano-scale solid electrolyte precursor, which comprises:
a reaction kettle body; the stirring device, the heating device and the feeding controller are arranged on the reaction kettle body; the stirring device is used for stirring reaction materials, the heating device is used for controlling the temperature in the reaction process, and the feeding controller is used for adding materials in the reaction process;
a temperature sensor; the temperature sensor is arranged in the reaction kettle body and used for monitoring the reaction temperature and transmitting a temperature signal to the heating device, and the heating device is turned on or off according to the temperature signal;
a pH sensor; the pH sensor is arranged in the reaction kettle body and used for monitoring the pH value of the reaction and transmitting the pH value signal to the charging controller, and the charging controller adds an acid-base regulator according to the pH value signal.
For the purpose of understanding the technical scheme of the present invention, the operation principle of the continuous reactor will be explained.
Firstly, in the preparation stage, reaction raw materials are respectively added into feed inlets of the continuous reactor, and the number of the feed inlets is matched with the types of the reaction raw materials.
Secondly, with the beginning of the reaction, the charging controller puts corresponding raw materials (including solvent, dispersant, acid-base modifier, monovalent element salts, trivalent element salts, tetravalent element salts and the like) into the reaction kettle body according to a parameter proportion set in advance, and at the moment, the stirring device stirs, so that the reaction system is more uniform; and meanwhile, the heating device heats to provide necessary temperature for the reaction.
In addition, the temperature sensor and the pH sensor can monitor the temperature and the pH value of the reaction system in real time while the reaction is carried out. It is emphasized that if the system pH is too low (acidity is too high) during the reaction, the pH sensor can transmit a signal of "acidity is too high, and alkaline agent needs to be added" to the feeding controller, and the feeding controller further regulates and controls the alkaline agent in the feeding port to be added to the system until the pH value meets the requirement; similarly, when the pH value of the system is too high (alkalinity is too high) in the reaction process, reverse regulation is also carried out according to the logic. And the adjustment for the temperature is: if the temperature in the reaction process is too high, the temperature sensor can transmit a signal of 'temperature is too high and temperature needs to be reduced' to the heating device, and the heating device can reduce the heating power or be directly closed, so that the reaction system is cooled until the temperature meets the requirement; similarly, when the system temperature is too low in the reaction process, reverse regulation is also carried out according to the logic.
And finally, directly discharging when the temperature of the system is balanced after the reaction is finished.
Preferably, the outer side of the reaction kettle body is wrapped with a cooling liquid interlayer, and the cooling liquid interlayer can be filled with cooling liquid; the cooling liquid interlayer is communicated with a cooling inlet and a cooling outlet.
Preferably, the stirring device comprises a stirring driving device and a stirring execution device; the stirring driving device is arranged at the top of the reaction kettle body, and the stirring executing device is arranged in the reaction kettle body; the output end of the stirring driving device is connected with the stirring execution device through a stirring rod.
Preferably, the stirring driving device is provided with a driving cooling liquid inlet and a driving cooling liquid outlet; the driving cooling liquid inlet and the driving cooling liquid outlet are respectively used for introducing and flowing out cooling liquid, and the cooling liquid is used for cooling the stirring driving device.
Preferably, the stirring executing device comprises a plurality of groups of stirring paddles which are sequentially arranged from top to bottom, and the stirring paddles are vertically arranged along the direction of the stirring rod.
Preferably, the heating device is a microwave generator.
Preferably, the microwave generator comprises a plurality of groups of microwave generating units, and the microwave generating units are circumferentially and uniformly arranged on the inner side of the reaction kettle body.
Preferably, the continuous reactor further comprises a display; the display is connected with the temperature sensor and the pH sensor and is used for displaying the reaction temperature and the pH value.
Preferably, the outlet at the bottom of the continuous reactor further comprises a discharge filtering device for filtering impurities in the feed liquid during discharge.
Preferably, the bottom of the continuous reactor further comprises a lifting foot rest for adjusting the height of the continuous reactor.
The utility model has the beneficial effects that:
the continuous reactor for synthesizing the high-crystallinity nano-scale solid electrolyte precursor by microwave can monitor the temperature and the pH value of a reaction system in real time, transmit signals to the heating device and the feeding controller, automatically and accurately adjust the temperature and the pH value in the reaction process, and enable the reaction to be carried out smoothly.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the structure of a continuous reactor according to the present invention;
FIG. 2 is a schematic top view of a reactor body according to the present invention;
FIG. 3 is a schematic structural view of a stirring paddle according to the present invention;
FIG. 4 is a schematic diagram of the construction of the discharge filter apparatus of the present invention.
Reference numbers in the figures:
1-a continuous reactor; 11-a reaction kettle body; 111-coolant interlayer; 112-cooling inlet; 113-a cooling outlet; 12-a stirring device; 121-stirring driving means; 1211 — drive coolant inlet; 1212-driving coolant outlet; 122-a stirring paddle; 13-a temperature sensor; 14-a pH sensor; 15-a heating device; 151-a microwave generating unit; 16-a feed controller; 17-a display; 18-a discharge filtration unit; 19-lifting foot stool.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the utility model, and not restrictive of the full scope of the utility model. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
In addition, in the description of the present invention, it is to be understood that the terms "upper", "lower", "inside", "outside", "top", "bottom", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present application and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be configured and operated in a specific orientation, and thus, should not be construed as limiting the present application.
Example 1
Referring to fig. 1, the present embodiment provides a continuous reactor for synthesizing a highly-crystalline nanoscale solid-state electrolyte precursor, the continuous reactor 1 including:
a reaction kettle body 11; the stirring device 12, the heating device 15 and the feeding controller 16 are arranged on the reaction kettle body 11; the stirring device 12 is used for stirring reaction materials, the heating device 15 is used for controlling the temperature in the reaction process, and the feeding controller 16 is used for adding materials in the reaction process;
a temperature sensor 13; the temperature sensor 13 is arranged inside the reaction kettle body 11, the temperature sensor 13 is used for monitoring the reaction temperature and transmitting a temperature signal to the heating device 15, and the heating device 15 is turned on or off according to the temperature signal;
a pH sensor 14; the pH sensor 14 is arranged inside the reaction kettle body 11, the pH sensor 14 is used for monitoring the reaction pH value and transmitting the pH value signal to the charging controller 16, and the charging controller 16 adds an acid-base regulator according to the pH value signal.
Example 2
On the basis of the example 1, as an alternative implementation manner, referring to fig. 2, a cooling liquid interlayer 111 is wrapped on the outer side of the reaction kettle body 11, and the cooling liquid interlayer can be filled with cooling liquid; the cooling liquid interlayer 111 is provided with a cooling inlet 112 and a cooling outlet 113 in a communication manner. In actual operation, the size of the reaction kettle body 11 can be changed with different reaction requirements. When the reaction kettle body 11 is large and the reaction temperature is too high and needs rapid cooling, the effect is limited only by the method of closing the heating device. Therefore, the cooling liquid interlayer 111, the cooling inlet 112 and the cooling outlet 113 are arranged on the outer side of the reaction kettle body 11, and the effect of rapid cooling is achieved by introducing external cooling liquid.
As an alternative embodiment, referring to fig. 1, the stirring device 12 includes a stirring driving device 121 and a stirring execution device; the stirring driving device 121 is arranged at the top of the reaction kettle body 11, and the stirring executing device is arranged inside the reaction kettle body 11; the output end of the stirring driving device 121 is connected to the stirring executing device through a stirring rod. The stirring driving device 121 may be a motor, and the motor generates a driving force to drive the stirring executing device to stir through the stirring rod.
As an alternative embodiment, referring to fig. 1, the stirring driving device 121 is provided with a driving cooling liquid inlet 1211 and a driving cooling liquid outlet 1212; the driving cooling liquid inlet 1211 and the driving cooling liquid outlet 1212 respectively introduce and flow out cooling liquid, and the cooling liquid is used for cooling the stirring driving device 121. In the actual operation process, the whole chemical reaction process needs to be in a stirring environment, and long-time work can make the stirring driving device 121 be in a high-temperature state, and if the temperature is not lowered in time, mechanical parts can be damaged. Therefore, the stirring driving device 121 is provided with a driving cooling liquid inlet 1211 and a driving cooling liquid outlet 1212, and the stirring driving device 121 can be in a better working environment by adding cooling liquid, so that the service life is prolonged.
As an optional implementation manner, referring to fig. 3, the stirring executing device includes a plurality of groups of stirring paddles 122 sequentially arranged from top to bottom, and the adjacent stirring paddles 122 are vertically arranged along the direction of the stirring rod. So set up, can make the stirring process more even to increase the lifting surface area of reaction system, be favorable to going on of reaction.
As an alternative embodiment, the heating device15 is a microwave generator. As the name implies, a microwave generator is capable of generating microwaves, which are electromagnetic waves propagating in a straight line and having a frequency of 300MHz to 300 GHz. The microwave absorbing capacity of a substance is mainly determined by the dielectric loss factor of the substance, the substance with large dielectric loss factor has strong microwave absorbing capacity, for example, water molecules belong to polar molecules, the dielectric constant is large, the dielectric loss factor is also large, and the substance has strong microwave absorbing capacity; while some solid substances, e.g. NiO, CuO, Fe3O4Or carbon black, etc., which can absorb microwave energy strongly and be heated rapidly, and some substances, such as CaO, Fe2O3Or TiO2Etc., the microwave energy is hardly absorbed, and the temperature rise range is small. When the microwave penetrates through an object, a directional electromagnetic field is attached, so that polar molecules are always arranged in the direction of the electromagnetic field under the action of the electric field, the molecules are called to be polarized, and because the microwave is an electromagnetic field oscillating for hundreds of millions of times per second, the arrangement direction of the molecules is changed for hundreds of millions of times per second when the microwave is placed in the electromagnetic field, so that a large number of molecules absorb the energy of the microwave and rotate violently at high frequency, a large amount of internal energy is generated, and the temperature of the object is increased. According to the principle, the NASICON precursor can be quickly and regularly arranged and uniformly reacted under the microwave heating, the average grain diameter of the obtained product is smaller, and Li in the crystal+The conduction path is more unobstructed.
As an alternative embodiment, referring to fig. 2, the microwave generator includes a plurality of sets of microwave generating units 151, and the microwave generating units 151 are circumferentially and uniformly arranged inside the reaction kettle body 11. In actual operation, in order to prevent the interference of microwave to communication, the microwave generation frequency is 915MHz and 2450MHz, wherein the 2450MHz is mainly used for household cooking utensils, and the 915MHz is used for industries such as drying, disinfection and the like, medical industries and the like. The frequency emitted by the microwave generating unit 151 is 915MHz, so that the microwave generating unit has better penetration distance and output power of 1000-2500W. In order to make the heating more uniform, the microwave generating units 151 are circumferentially and uniformly disposed inside the reaction kettle body 11. For example, 6 groups of the microwave generating units 151 are selected, and the microwave generating units are sequentially numbered as a, b, c, d, e, and f according to the clockwise number, so that the microwave generating units are arranged according to a regular six-sided layout, when heating is required, the microwave generating units numbered as a, c, and e or the microwave generating units numbered as b, d, and f are simultaneously turned on (turned on at intervals), if a, c, and e are turned on first, then turned off after heating for 20s, and then turned on b, d, and f, and the process is repeated until the temperature reaches a set value. The intermittent heating at different angles can also increase the uniformity of the energy received by the material.
As an alternative embodiment, with reference to fig. 1, the continuous reactor 1 further comprises a display 17; the display 17 is connected with the temperature sensor 13 and the pH sensor 14 and is used for displaying the reaction temperature and the pH value. The display 17 is arranged to observe the reaction state of the system in real time, so that the emergency situation can be handled in the first time.
As an alternative embodiment, with reference to fig. 4, the outlet at the bottom of the continuous reactor 1 further comprises an outlet filtering device 18 for filtering feed liquid impurities during outlet. When the reaction is finished and the material is discharged, the discharging and filtering device 18 can filter impurities and purify the material liquid.
As an alternative embodiment, referring to fig. 1, the bottom of the continuous reactor 1 further comprises a liftable foot rest 19 for height adjustment of the continuous reactor 1. The foot rests enable the continuous reactor 1 to be more stable; in addition, when the reaction is finished and the material is discharged, the foot rest can be lifted, and the material outlet is higher than the collecting barrel for transfer, so that the material liquid can be collected more conveniently.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A continuous reactor for the synthesis of highly crystalline nanoscale solid-state electrolyte precursors, characterized in that the continuous reactor (1) comprises:
a reaction kettle body (11); the stirring device (12), the heating device (15) and the feeding controller (16) are arranged on the reaction kettle body (11); the stirring device (12) is used for stirring reaction materials, the heating device (15) is used for controlling the temperature in the reaction process, and the feeding controller (16) is used for adding materials in the reaction process;
a temperature sensor (13); the temperature sensor (13) is arranged inside the reaction kettle body (11), the temperature sensor (13) is used for monitoring the reaction temperature and transmitting a temperature signal to the heating device (15), and the heating device (15) is opened or closed according to the temperature signal;
a pH sensor (14); the pH sensor (14) is arranged inside the reaction kettle body (11), the pH sensor (14) is used for monitoring the reaction pH value and transmitting the pH value signal to the charging controller (16), and the charging controller (16) adds an acid-base regulator according to the pH value signal.
2. The continuous reactor for synthesizing the high-crystallinity nanoscale solid electrolyte precursor as claimed in claim 1, wherein the outer side of the reaction kettle body (11) is wrapped with a cooling liquid interlayer (111), and the cooling liquid interlayer can be filled with cooling liquid; the cooling liquid interlayer (111) is communicated with a cooling inlet (112) and a cooling outlet (113).
3. The continuous reactor for synthesizing a highly-crystalline nanoscale solid-state electrolyte precursor according to claim 1, wherein the stirring device (12) comprises a stirring driving device (121) and a stirring execution device; the stirring driving device (121) is arranged at the top of the reaction kettle body (11), and the stirring executing device is arranged inside the reaction kettle body (11); the output end of the stirring driving device (121) is connected with the stirring execution device through a stirring rod.
4. The continuous reactor for synthesizing highly-crystallized nanoscale solid-state electrolyte precursor as claimed in claim 3, wherein said stirring driving device (121) is provided with a driving cooling liquid inlet (1211) and a driving cooling liquid outlet (1212); the driving cooling liquid inlet (1211) and the driving cooling liquid outlet (1212) respectively introduce and flow out cooling liquid, and the cooling liquid is used for cooling the stirring driving device (121).
5. The continuous reactor for synthesizing the high-crystallinity nanoscale solid-state electrolyte precursor as claimed in claim 3, wherein the stirring actuator comprises a plurality of groups of stirring paddles (122) arranged from top to bottom, and the stirring paddles (122) are arranged vertically along the direction of the stirring rod.
6. The continuous reactor for synthesizing highly crystalline nanoscale solid electrolyte precursor according to claim 1, wherein the heating device (15) is a microwave generator.
7. The continuous reactor for synthesizing the highly-crystallized nanoscale solid-state electrolyte precursor according to claim 6, wherein the microwave generator comprises multiple groups of microwave generating units (151), and the microwave generating units (151) are circumferentially and uniformly arranged inside the reaction kettle body (11).
8. The continuous reactor for synthesizing highly crystalline nanoscale solid-state electrolyte precursor according to claim 1, wherein said continuous reactor (1) further comprises a display (17); the display (17) is connected with the temperature sensor (13) and the pH sensor (14) and is used for displaying the reaction temperature and the pH value.
9. The continuous reactor for synthesizing the highly-crystallized nano-scale solid electrolyte precursor according to claim 1, wherein the outlet at the bottom of the continuous reactor (1) further comprises a discharge filtering device (18) for filtering impurities in the feed liquid during discharge.
10. The continuous reactor for synthesizing highly crystalline nanoscale solid-state electrolyte precursor according to claim 1, wherein the bottom of the continuous reactor (1) further comprises a liftable foot rest (19) for height adjustment of the continuous reactor (1).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114432994A (en) * | 2022-01-28 | 2022-05-06 | 瑟瑞米(洛阳)新能源科技有限公司 | Continuous reactor for synthesizing high-crystallinity nano-scale solid electrolyte precursor and synthesis method |
| CN117234266A (en) * | 2023-11-13 | 2023-12-15 | 长沙矿冶研究院有限责任公司 | Ternary precursor reaction kettle reaction reverse selectivity control method and system |
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- 2022-01-28 CN CN202220243746.5U patent/CN216799833U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114432994A (en) * | 2022-01-28 | 2022-05-06 | 瑟瑞米(洛阳)新能源科技有限公司 | Continuous reactor for synthesizing high-crystallinity nano-scale solid electrolyte precursor and synthesis method |
| CN117234266A (en) * | 2023-11-13 | 2023-12-15 | 长沙矿冶研究院有限责任公司 | Ternary precursor reaction kettle reaction reverse selectivity control method and system |
| CN117234266B (en) * | 2023-11-13 | 2024-03-22 | 长沙矿冶研究院有限责任公司 | Ternary precursor reaction kettle reaction reverse selectivity control method and system |
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