Ternary precursor reaction kettle anti-oxidation system

Abstract

The utility model discloses an anti-oxidation system of a ternary precursor reaction kettle, and belongs to the technical field of reaction kettles. The reaction kettle comprises a reaction kettle body, a gas inlet pipe, a regulating valve, a stirrer, an atmosphere analysis system, a gas sampling pipe, a sucking pump and a switch valve. In order to meet the standard that the inert gas content can fully prevent materials in the reaction kettle body from being oxidized, preset conditions are set in the control system. Gas in the reaction kettle body is collected and monitored through the atmosphere analysis system and the sucking pump, gas content information is generated after the content of inert gas is obtained, and the control system obtains the gas content information to know whether the content of the inert gas in the reaction kettle body meets set preset conditions or not. The gas inlet amount of the inert gas is adjusted and controlled by adjusting and controlling the adjusting valve, so that the actual inert gas content in the reaction kettle body can be kept to be the preset condition, and waste caused by excessive inert gas introduction can be prevented while the anti-oxidation of materials is guaranteed.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of reaction kettle, especially relates to a ternary precursor reaction kettle anti -oxidation system. BACKGROUND

[0002] Lithium ion battery is mainly composed of four major materials such as positive electrode, negative electrode, electrolyte and diaphragm. Positive electrode material is the core component of lithium ion battery, and has a direct influence on many core performance indexes of lithium ion battery, including capacity, service life, rate, safety, etc. Positive electrode material includes lithium cobaltate, lithium manganate, ternary positive electrode, lithium iron phosphate, etc. Ternary precursor is the main raw material of ternary positive electrode, and the quality of ternary precursor directly affects the performance of ternary positive electrode material.

[0003] In addition to the performance such as main content, particle size and tap density, the morphology and specific surface area of ternary precursor also affect the performance of ternary positive electrode material, and the oxidation in the production process of ternary precursor will affect the morphology and specific surface area of ternary precursor. At present, most enterprises adopt the method of directly introducing inert gas into the reaction kettle to make inert environment exist in the reaction kettle, but if the inert gas content in the air above the material is too small, the material will still be oxidized. In order to better prevent the oxidation of the material, excessive inert gas such as nitrogen is often introduced into the reaction kettle, which easily leads to the problem of waste of inert gas. UTILITY MODEL CONTENT

[0004] The utility model aims at providing a kind of ternary precursor reaction kettle anti-oxidation system to solve one or more technical problems existing in prior art, at least provide a beneficial choice or create conditions.

[0005] The technical scheme adopted to solve the above technical problems is as follows: a kind of ternary precursor reaction kettle anti-oxidation system, comprising: reaction kettle body, is communicated with inlet pipe, the inert gas is connected to the inlet pipe, the inlet pipe is equipped with regulating valve for adjusting the inlet amount of the inert gas, the reaction kettle body is equipped with agitator for stirring internal liquid;Atmosphere analysis system is connected with gas sampling pipe, the gas sampling pipe is successively equipped with air pump and switch valve, and finally communicated in the reaction kettle body, the atmosphere analysis system can control the start-stop of the air pump and the switch valve, the atmosphere analysis system is used to monitor the content of the inert gas in the reaction kettle body and generate gas content information;Control system is used to obtain the gas content information and control the opening of the regulating valve according to preset condition.

[0006] The technical scheme has at least the following beneficial effects: The preset condition is set in the control system, and the preset condition is a standard that satisfies the inert gas content capable of fully preventing the material in the reaction kettle body from being oxidized. The gas in the reaction kettle body is collected and monitored by the atmosphere analysis system and the air pump, the inert gas content is obtained to generate gas content information, the control system learns whether the inert gas content in the reaction kettle body meets the preset condition by acquiring the gas content information, and the regulating valve is adjusted to adjust the inert gas inlet amount, so that the actual inert gas content in the reaction kettle body can be maintained as the preset preset condition, and thus the waste caused by excessive inert gas inlet can be prevented while ensuring the oxidation prevention of the material.

[0007] As a further improvement of the above technical scheme, the reaction kettle oxidation prevention system further comprises a vortex breaker, the vortex breaker comprises a support frame installed in the reaction kettle body and a vortex plate installed on the support frame, and the vortex plate is inserted into the liquid surface of the internal liquid and used to hinder the vortex movement of the liquid surface. When the internal liquid is stirred by the stirrer, vortex movement is easily generated, which causes the material to be more easily oxidized. The vortex plate inserted into the liquid surface of the internal liquid can hinder the vortex movement of the liquid surface of the internal liquid, thereby reducing the problem of large vortex of the liquid surface of the internal liquid in the reaction kettle body caused by the increase of stirring intensity, improving the quality of the product.

[0008] As a further improvement of the above technical scheme, the number of vortex breakers is multiple, and the multiple vortex breakers are annularly distributed around the stirring center line of the stirrer. The multiple annularly distributed vortex breakers hinder the vortex movement of multiple parts of the internal liquid, which can improve the effect of hindering the vortex movement of the internal liquid and further prevent the internal liquid from being easily oxidized due to vortex movement. In addition, the liquid surface of the internal liquid can be kept in a relatively stable and uniform state after the vortex movement is hindered.

[0009] As a further improvement of the above technical scheme, a rotating shaft and a limiting member are installed between the support frame and the vortex plate, the length direction of the rotating shaft is parallel to the stirring center line of the stirrer, the vortex plate can rotate around the rotating shaft relative to the support frame to adjust the angular position of the vortex plate, and the limiting member is used to fix the angular position of the adjusted vortex plate. When the vortex plate rotates relative to the support frame, the angular position of the vortex plate when hindering the vortex movement of the internal liquid can be changed, thereby affecting the effect of hindering the vortex movement. Therefore, the angular position of the vortex plate can be adjusted according to actual needs to achieve a better oxidation prevention effect caused by hindering the vortex movement.

[0010] As a further improvement of the above technical solution, the rotating shaft is a fixed rod penetrating through the support frame and the vortex breaking plate, and the limiting member is a fixed nut, which is threadedly connected with the fixed rod. When the fixed nut is screwed, the fixed nut and the fixed rod can clamp the support frame and the vortex breaking plate to limit the rotation of the vortex breaking plate relative to the support frame. By providing the fixed rod and the fixed nut, the vortex breaking plate can be rotatably installed on the support frame, and the angle position of the vortex breaking plate can be adjusted by loosening and tightening the fixed nut, which is simple in structure and convenient to install and adjust.

[0011] As a further improvement of the above technical solution, the reaction kettle anti-oxidation system further comprises a gas mixer installed at the top of the reaction kettle body, the gas mixer is provided with a main gas inlet communicated with the gas inlet pipe and an annular channel communicated with the main gas inlet, a plurality of shunt gas paths are formed in the gas mixer and are arranged in a ring around the stirring center line of the stirrer, one end of the shunt gas path is a gas path gas inlet communicated with the annular channel, and the other end is a gas path gas outlet communicated with the inside of the reaction kettle body. When the inert gas is introduced from the gas inlet pipe, it enters the annular channel from the main gas inlet, is dispersed into each shunt gas path, and is sprayed out from the plurality of shunt gas paths, forming a strong gas convection in the reaction kettle body, so that the atmosphere in the reaction kettle body is quickly mixed and uniform, and the content of inert gas in the reaction kettle body is uniformly controlled. In addition, it can also reduce the situation that the sampling and detection results exist lag or error due to uneven atmosphere, ensure the accuracy of monitoring, prevent the frequent movement of inert gas and the loss of inert gas caused thereby.

[0012] As a further improvement of the above technical solution, the directions of the lines connecting the two ends of the plurality of shunt gas paths and the circumferential radius direction of the annular channel form an included angle β greater than 0 and less than 90 degrees, the shunt gas paths are inclined relative to the circumferential radius direction of the annular channel, and one end of the gas path gas outlet of the shunt gas path is bent towards the stirring center line direction of the stirrer. It can prevent the situation that the shunt gas paths near the main gas inlet shunt out inert gas too fast, resulting in a large difference in inert gas flow rate between the shunt gas paths, improve the uniformity of inert gas shunting, and further improve the mixing effect of inert gas. In the limited space of the gas mixer, the length of the shunt gas path can be extended and the counterflow effect of the sprayed gas can be ensured to improve the shunting effect of the inert gas.

[0013] As a further improvement of the above technical solution, the cross-sectional area of the gas path gas inlet is greater than the cross-sectional area of the gas path gas outlet. Thus, the speed of inert gas spraying can be increased to accelerate the mixing of inert gas.

[0014] As a further improvement of the above technical solution, the gas sampling pipe is further provided with a dryer and an ammonia gas absorber, the dryer is arranged between the switch valve and the air pump, and the ammonia gas absorber is arranged between the dryer and the air pump. The dryer and the ammonia gas absorber can remove water vapor and ammonia gas in the sampling gas respectively, so that the monitoring process of the atmosphere analysis system can be facilitated.

[0015] As a further improvement of the above technical solution, the gas sampling pipe is further provided with a first filter and a second filter, the first filter is arranged between the switch valve and the dryer, and the second filter is arranged between the air pump and the atmosphere analysis system. The first filter can filter out some particulate impurities in the sampling gas, so as to facilitate subsequent drying and ammonia gas absorption treatment, and the second filter can further filter out some particulate impurities in the sampling gas, so as to prevent the particulate impurities from affecting the monitoring result of the atmosphere analysis system and damaging the internal structure of the atmosphere analysis system. BRIEF DESCRIPTION OF DRAWINGS

[0016] The above and / or additional aspects and advantages of the present application will become apparent and more readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings in which:

[0017] Figure 1 is a whole schematic view of the embodiment of the present application;

[0018] Figure 2 is a ring distribution schematic view of the vortex breaker in the embodiment of the present application;

[0019] Figure 3 is a structure schematic view of the vortex breaker in the embodiment of the present application;

[0020] Figure 4 is an exploded structure schematic view of the vortex breaker in the embodiment of the present application;

[0021] Figure 5 is an exploded structure schematic view of the limiting member in the embodiment of the present application;

[0022] Figure 6 is a structure schematic view of the gas mixer in the embodiment of the present application;

[0023] Figure 7 is a structure schematic view of the reaction kettle of the prior art;

[0024] Figure 8 is a SEM image of the reaction kettle slurry of Example 1;

[0025] Figure 9 is a SEM image of the reaction kettle slurry of Comparative Example 1;

[0026] Figure 10This is a SEM image of the reaction vessel slurry from Example 2;

[0027] Figure 11 This is a SEM image of the reaction slurry in Comparative Example 2.

[0028] 1. Reactor body; 2. Stirrer; 3. Vortex breaker; 31. Support frame; 32. Vortex breaker plate; 33. Fixing rod; 34. Fixing nut; 4. Gas mixer; 41. Main air inlet; 42. Diverter gas path; 43. Gas path inlet; 44. Gas path outlet; 5. Switch valve; 6. First filter; 7. Dryer; 8. Gas sampling tube; 9. Ammonia absorber; 10. Vacuum pump; 11. Second filter; 12. Atmosphere analysis system; 13. Exhaust pipe; 14. Control system; 15. Regulating valve; 16. Inlet pipe; 18. Manual ball valve; 19. Nitrogen inlet pipe. Detailed Implementation

[0029] The embodiments of this utility model are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this utility model, and should not be construed as limiting this utility model.

[0030] In the description of this utility model, it should be understood that the directional descriptions, such as up, down, front, back, left, right, etc., indicate the directional or positional relationship based on the directional or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0031] In the description of this utility model, "several" means one or more, "multiple" means two or more, "greater than," "less than," and "exceeding" are understood to exclude the stated number, while "above," "below," and "within" are understood to include the stated number. If "first" or "second" is used in the description, it is only for the purpose of distinguishing technical features and should not be construed as indicating or implying relative importance, or implicitly indicating the number of indicated technical features, or implicitly indicating the order of the indicated technical features.

[0032] In the description of this utility model, unless otherwise explicitly defined, terms such as "setting," "installation," and "connection" should be interpreted broadly, and those skilled in the art can reasonably determine the specific meaning of the above terms in this utility model in conjunction with the specific content of the technical solution.

[0033] Reference Figures 1-6The oxidation prevention system of the ternary precursor reactor includes a reactor body 1, an atmosphere analysis system 12, and a control system 14. The reactor body 1 is equipped with a stirrer 2, which includes a motor and a stirring rod mounted on the motor's output end. The motor is mounted on the top of the reactor body 1, and the stirring rod is rotatably positioned inside the reactor body 1, arranged vertically, meaning the stirring center line of the stirrer 2 is a vertical line. The stirring rod can be rotated by driving the motor, thereby stirring the liquid contained within the reactor body 1.

[0034] An inlet pipe 16 is connected to the top of the reactor body 1. The end of the inlet pipe 16 away from the reactor body 1 is connected to an inert gas supply end, preferably nitrogen. A regulating valve 15 is installed on the inlet pipe 16. The regulating valve 15 can adjust the flow rate of the inlet pipe 16, thereby regulating the amount of inert gas entering the reactor body 1. The regulating valve 15 is preferably made of 304 stainless steel.

[0035] An atmosphere analysis system 12 is used to monitor the content of inert gas inside the reactor body 1. Preferably, the atmosphere analysis system 12 is a multi-atmosphere online analysis system. A gas sampling tube 8 is connected to the monitoring end of the atmosphere analysis system 12. The end of the gas sampling tube 8 furthest from the atmosphere analysis system 12 is connected to the interior of the reactor body 1, allowing gas inside the reactor body 1 to flow through the gas sampling tube 8 into the atmosphere analysis system 12 for monitoring the inert gas content. A vacuum pump 10 and a switching valve 5 are installed on the gas sampling tube 8. The switching valve 5 is located at the end of the gas sampling tube 8 closest to the reactor body 1, and is preferably made of 304 stainless steel. The vacuum pump 10 is located on the gas sampling tube 8 between the switching valve 5 and the atmosphere analysis system 12, and is preferably an oil-free, silent vacuum pump. Both the inlet pipe 16 and the gas sampling tube 8 are preferably 304 stainless steel mirror-polished pipes.

[0036] The atmosphere analysis system 12 is communicatively connected to the vacuum pump 10 and the switching valve 5. When the atmosphere analysis system 12 needs to perform detection, by controlling the vacuum pump 10 to open and the switching valve 5 to open, the gas inside the reactor body 1 can be drawn into the atmosphere analysis system 12 for monitoring. After monitoring the sampled gas, the atmosphere analysis system 12 obtains relevant information such as the content and concentration of inert gases in the sampled gas and generates gas content information. The atmosphere analysis system 12 is equipped with an exhaust pipe 13 for discharging the sampled gas that has already been tested.

[0037] The control system 14 is communicatively connected to the atmosphere analysis system 12, such as via a data cable or a wireless local area network. The control system 14 is also communicatively connected to the regulating valve 15, enabling the control system 14 to adjust the opening degree of the regulating valve 15, such as via a data cable or a wireless local area network.

[0038] The control system 14 is configured with preset conditions, such as a standard content of inert gas sufficient to prevent oxidation of materials in the reactor body, like a standard nitrogen concentration in the reactor. The gas content information generated by the atmosphere analysis system 12 is sent to the control system 14. After acquiring the gas content information, the control system 14 compares the preset conditions with the gas content information, generates a control signal, and sends it to the regulating valve 15. Upon receiving the control signal, the regulating valve 15 adjusts its opening, thereby controlling the amount of inert gas introduced into the reactor body 1. This maintains a standard content of inert gas in the reactor body 1, ensuring that the materials are sufficiently protected from oxidation while minimizing waste caused by excessive inert gas intake.

[0039] The gas sampling tube 8 is also equipped with a dryer 7, which is located on the gas sampling tube 8 between the switching valve 5 and the suction pump 10. The dryer 7 contains a desiccant, preferably silica gel, which can absorb water vapor to remove water vapor from the sampled gas. At the same time, it can be recycled and reused, resulting in low operating costs.

[0040] The gas sampling tube 8 is also equipped with an ammonia absorber 9, which is located on the gas sampling tube 8 between the dryer 7 and the pump 10. The ammonia absorber 9 contains an ammonia removal agent, preferably anhydrous calcium chloride, which can absorb ammonia to remove ammonia from the sampled gas.

[0041] The gas sampling tube 8 is also equipped with a first filter 6, which is located on the gas sampling tube 8 between the switching valve 5 and the dryer 7. The gas sampling tube 8 is also equipped with a second filter 11, which is located on the gas sampling tube 8 between the suction pump 10 and the atmosphere analysis system 12. Both the first filter 6 and the second filter 11 are preferably precision filters, with the pore size of the precision filter element preferably less than 0.3 micrometers, and the material of the precision filter element preferably being PP material.

[0042] Furthermore, the anti-oxidation system for the reactor in this embodiment also includes a vortex breaker 3. The vortex breaker 3 includes a support frame 31 and a vortex-breaking plate 32. The support frame 31 is installed inside the reactor body 1, and the vortex-breaking plate 32 is installed on the support frame 31. The vortex-breaking plate 32 is inserted into the liquid surface of the internal liquid, such that two-thirds of the vortex-breaking plate 32 is below the liquid surface and one-third is above the liquid surface. When the internal liquid in the reactor body 1 is stirred by the stirrer 2, a vortex motion is generated. The vortex-breaking plate 32 can hinder the vortex motion of the internal liquid, thereby reducing the vortex on the surface of the internal liquid, solving the problem of easy oxidation of the internal liquid caused by the large vortex on the surface of the internal liquid due to the increased stirring intensity, and improving the quality of the product.

[0043] Specifically, the support frame 31 consists of two vertically distributed vertical rods and two horizontal rods connecting the two vertical rods. The tops of the two vertical rods are installed at the inner top position of the reactor body 1, thus allowing the support frame 31 to be installed inside the reactor body 1. The vortex-breaking plate 32 has a rotating shaft passing through it vertically, with both ends of the rotating shaft installed on the two horizontal rods respectively. That is, the length direction of the rotating shaft is parallel to the stirring center line of the reactor body 1. The vortex-breaking plate 32 can rotate relative to the support frame 31 around the center line of the rotating shaft, thereby changing the angular position of the vortex-breaking plate 32. A limiting member is installed between the support frame 31 and the vortex-breaking plate 32 to limit the angular position of the vortex-breaking plate 32. That is, both the support frame 31 and the vortex-breaking plate 32 are vertical planar structures, and an included angle α is formed between the support frame 31 and the vortex-breaking plate 32 on the horizontal plane. The limiting member can limit the included angle α to a fixed state.

[0044] Specifically, the rotating shaft is set as a fixed rod 33. One end of the fixed rod 33 has a large head, and the other end has a smaller rod. The rod of the fixed rod 33 passes vertically through the crossbar below the support frame 31, then through the middle of the vortex-breaking plate 32, and finally through the crossbar above the support frame 31. It can be understood that the length of the fixed rod 33 is parallel to the stirring center line of the reactor body 1. The limiting component is a fixing nut 34, which is threaded onto the top of the fixed rod 33, i.e., the end of the rod away from the head. When the fixing nut 34 is tightened, it clamps the two crossbars with the head of the fixed rod 33, thus clamping the vortex-breaking plate 32. This keeps the angle of the vortex-breaking plate 32 fixed, ensuring that it has sufficient support to impede the vortex movement of the internal liquid.

[0045] When the vortex-breaking plate 32 rotates relative to the support frame 31, its angular position in hindering the movement of the internal liquid vortex can be changed, thereby affecting the effect of hindering vortex movement. Therefore, the angular position of the vortex-breaking plate 32 can be adjusted according to actual needs to achieve a better anti-oxidation effect brought about by hindering vortex movement.

[0046] The gap between the two horizontal bars of the support frame 31 is equal to or slightly greater than the height of the vortex-breaking plate 32, allowing the vortex-breaking plate 32 to be embedded between the two horizontal bars. The gap between the two vertical bars is greater than or much greater than the thickness of the vortex-breaking plate 32, allowing the included angle α to be adjusted within a range of 10°-170°. The vortex-breaking plate 32 is provided with intersecting reinforcing ribs to prevent bending due to vigorous stirring. The tops of the two vertical bars of the support frame 31 can be directly fixed to the inner top of the reactor body 1 by welding, or they can be detachably installed on the inner top of the reactor body 1 by bolts.

[0047] In other embodiments, the limiting element may also be a screw threaded onto the vortex-breaking plate 32. After the screw is screwed into the vortex-breaking plate 32, it abuts against the rotating shaft, thereby limiting the relative rotation of the vortex-breaking plate 32 and fixing the angular position of the vortex-breaking plate 32.

[0048] The agitator 3 comprises eight vortex breakers 3, which are evenly distributed around the stirring center line of the agitator 2. These multiple vortex breakers 3 impede the vortex motion of the internal liquid at various points, improving the effectiveness of this impediment and further preventing oxidation caused by vortex motion. Furthermore, they help maintain a relatively stable and uniform liquid surface after impeding vortex motion. In other embodiments, the number of vortex breakers 3 can be four to seven.

[0049] Furthermore, the anti-oxidation system of the reactor in this embodiment also includes a gas mixer 4. The gas mixer 4 is an annular cylindrical structure and is installed at the inner top of the reactor body 1. The gas mixer 4 is provided with a main air inlet 41 and an independent annular channel. One end of the air inlet pipe 16 connected to the reactor body 1 is connected to the main air inlet 41. The main air inlet 41 is connected to the annular channel. Six branch gas paths 42 are also provided inside the gas mixer 4. The six branch gas paths 42 are evenly distributed around the stirring center line of the stirrer 2. The two ends of the branch gas paths 42 are respectively the gas path inlet 43 and the gas path outlet 44. The cross-sectional area of ​​the branch gas path 42, that is, the cross-sectional area perpendicular to the gas flow direction, gradually decreases from the gas path inlet 43 to the gas path outlet 44, so that the cross-sectional area of ​​the gas path inlet 43 is larger than the cross-sectional area of ​​the gas path outlet 44, so as to increase the speed of inert gas ejection and accelerate the mixing of inert gas. The gas inlet 43 is connected to the interior of the annular channel, and the gas outlet 44 extends through the inner wall of the gas mixer 4 and is connected to the interior of the reactor body 1.

[0050] After the inert gas enters the main inlet 41 through the inlet pipe 16, it disperses within the annular channel and is evenly sprayed into the interior of the reactor body 1 through the six branch gas paths 42. This creates intense gas convection within the reactor body 1, rapidly and uniformly mixing the atmosphere and controlling the inert gas content. Furthermore, this reduces lag or errors in sampling and detection results caused by uneven atmosphere, ensuring monitoring accuracy and preventing frequent adjustments to the inert gas and the resulting loss of inert gas.

[0051] Specifically, each of the six branch gas paths 42 forms an angle β greater than 0 and less than 90 degrees with the circumferential radius of the annular channel, making the branch gas paths 42 inclined relative to the circumferential radius of the annular channel. This extends the length of the branch gas paths 42, improves their guiding properties, and prevents the branch gas paths 42 near the main air inlet 41 from excessively diverting inert gas, thus preventing excessive differences in inert gas flow rates between the branch gas paths 42. This improves the uniformity of inert gas distribution and, consequently, enhances the mixing effect of the inert gas.

[0052] All six gas distribution paths 42 are curved, with the middle section of each path protruding in an inclined direction. Specifically, one end of the gas outlet 44 of each path is curved towards the stirring centerline of the stirrer 2 (i.e., the centerline of the annular channel). This allows the gas flowing through the gas distribution paths 42 to be guided to a position closer to the center of the reactor body 1, balancing the effect of the inclined arrangement of the gas distribution paths 42 causing the flow direction to deviate from the center of the reactor body 1. This achieves the extension of the gas distribution paths 42 within the limited space of the gas mixer 4 and ensures the counter-current effect of the ejected gas, thereby improving the diversion effect of the inert gas. In other embodiments, four, five, seven, or eight gas distribution paths 42 may also be provided.

[0053] Taking nitrogen as the inert gas, the specific manual workflow of the anti-oxidation system for a ternary precursor reactor provided in this application embodiment is as follows:

[0054] Preliminary preparations: Set the included angle α between the support frame 31 and the vortex-breaking plate 32 of the vortex breaker 3 to 45°, and tighten and lock the fixing rod 33 and fixing nut 34. Inject slurry into the reactor body 1, slowly start the agitator and increase the stirring speed to the required speed. Observe the vortex situation on the liquid surface inside the reactor body 1. Increase the temperature and add ammonia to meet the process requirements. Connect the gas and electrical circuits and turn on the gas and electricity. Turn on the main switch of the nitrogen and compressed air sources. Set the nitrogen concentration standard of the reactor body in the control system 14 and set the program to manual.

[0055] First, click the sampling analysis button on the interface of the atmosphere analysis system 12. The atmosphere analysis system 12 transmits the sampling signal to the switch valve 5 and the vacuum pump 10 through the signal connection line. The switch valve 5 opens first, and then the vacuum pump 10 starts. The vacuum pump 10 extracts the gas above the liquid surface of the reactor body 1 through the gas sampling pipe 8.

[0056] The second step involves the extracted gas passing through the gas sampling tube 8, first through the switch valve 5, then through the first filter 6 to remove some particulate matter, and then through the dryer 7. The desiccant in the dryer 7 removes water vapor from the gas. The dried gas then passes through the ammonia absorber 9, where the ammonia remover removes ammonia from the gas. The remaining gas then passes through the vacuum pump 10, and then through the second filter 11 to further remove particulate matter. Finally, the gas enters the atmosphere analysis system 12. At the same time, the vacuum pump 10 and the switch valve 5 are manually shut off.

[0057] Third, click the analysis button on the atmosphere analysis system 12 to analyze the collected gas and obtain the nitrogen concentration in the gas. At the same time, click the exhaust button on the atmosphere analysis system 12 interface to discharge the analyzed gas to the outside through the exhaust pipe 13.

[0058] Fourth, based on the nitrogen concentration results, compare them with the nitrogen concentration standard required by the reactor body, click on the operation interface of the control system 14, set the opening size of the regulating valve 15, and the signal will be transmitted to the regulating valve 15 through the signal connection line to control the nitrogen to pass through the gas inlet pipe 16, and then enter the gas mixer 4 from the main inlet 41 of the gas mixer 4, and then enter from the gas inlet 43 of the multiple curved branch gas paths 42, and finally be quickly ejected from the gas outlet 44 of the multiple branch gas paths 42, forming a violent gas convection in the reactor body, so that the atmosphere in the reactor body is quickly and evenly mixed, and the nitrogen content in the reactor body 1 is uniformly controlled.

[0059] Fifth, the control room operators repeat the above operations at irregular intervals to sample, analyze, and regulate the atmosphere inside the reactor body 1.

[0060] Alternatively, both the control system and the atmosphere analysis system are equipped with automatic programs. The specific automatic workflow is as follows:

[0061] Preliminary preparations: Set the included angle α between the support frame 31 and the vortex-breaking plate 32 of the vortex breaker 3 to 90°, and tighten and lock the fixing rod 33 and fixing nut 34. Inject slurry into the reactor body 1, slowly start the agitator and increase the stirring speed to the required speed. Observe the vortex situation on the liquid surface inside the reactor body 1. Increase the temperature and add ammonia to meet the process requirements. Connect the gas and electrical circuits and turn on the gas and power. Turn on the main switch of the nitrogen and compressed air sources. Set the nitrogen concentration standard of the reactor body in the control system 14, set the program to automatic, and set the sampling and monitoring frequency.

[0062] First, click the sampling analysis button on the interface of the atmosphere analysis system 12, and at the same time set the program to "automatic". The atmosphere analysis system 12 transmits the sampling signal to the switch valve 5 and the vacuum pump 10 through the signal connection line. The switch valve 5 opens first, and then the vacuum pump 10 starts. The vacuum pump 10 extracts the gas above the liquid surface of the reactor body 1 through the gas sampling pipe 8.

[0063] In the second step, the extracted gas passes through the gas sampling tube 8, first through the switch valve 5, then through the first filter 6 to filter out some particulate matter in the gas, and then through the dryer 7. The desiccant in the dryer 7 removes water vapor from the gas. The dried gas then passes through the ammonia absorber 9. The ammonia remover in the ammonia absorber 9 removes ammonia from the gas. The remaining gas then passes through the vacuum pump 10, and then through the second filter 11 to further filter out particulate matter in the gas, and finally enters the atmosphere analysis system 12. At the same time, the vacuum pump 10 and the switch valve 5 are automatically shut off.

[0064] Third, the atmosphere analysis system 12 automatically analyzes the collected gas to obtain the nitrogen concentration in the gas, and then transmits this result to the control system 14 via a data cable. At the same time, the atmosphere analysis system 12 automatically discharges the analyzed gas to the outside through the exhaust pipe 13.

[0065] Fourth, after receiving the nitrogen concentration data from the atmosphere analysis system 12, the control system 14 transmits the operation signal to the regulating valve 15 through the signal connection line according to the nitrogen concentration standard set in the program. The regulating valve 15 adjusts the valve opening to control the nitrogen to pass through the gas inlet pipe 16, and then enter the gas mixer 4 from the main inlet 41 of the gas mixer 4. It then enters from the gas inlet 43 of the multiple curved branch gas paths 42, and finally is quickly ejected from the gas outlet 44 of the multiple curved branch gas paths 42, forming a violent gas convection in the reactor body, so that the atmosphere in the reactor body is quickly and evenly mixed, and the nitrogen content in the reactor body 1 is uniformly controlled.

[0066] Fifth, the program automatically samples, analyzes, and regulates the atmosphere inside the reactor body 1 periodically according to the set frequency.

[0067] Reference Figure 7 In the prior art, the reactor is connected to a nitrogen inlet pipe 19, and a manual ball valve 18 is installed on the nitrogen inlet pipe 19. The amount of nitrogen entering the reactor is controlled by manually adjusting the manual ball valve 18.

[0068] The manual workflow of this embodiment is set as Embodiment 1.

[0069] The automated workflow of this embodiment is set as Embodiment 2.

[0070] Comparative Example 1:

[0071] Reference Figure 7 Open the manual ball valve 18, and nitrogen gas enters the reactor through the nitrogen inlet pipe 19 to provide nitrogen protection for the materials in the reactor.

[0072] Comparative Example 2:

[0073] Reference Figure 7 Open the manual ball valve 18 halfway, and nitrogen gas enters the reactor through the nitrogen inlet pipe 19 to provide nitrogen protection for the materials in the reactor.

[0074] Figures 8-11 The SEM images after the above embodiments and comparative examples are shown below. The specific surface area of ​​the reactor slurry is shown in the following figures.

[0075] Tables 1 and 2. Comparative Example 1 above represents the technical solutions currently available on the market.

[0076]

[0077]

[0078] It is understandable that the SEM and specific surface area mentioned above are obtained from the ternary precursor through the reaction vessel slurry.

[0079] Reference Figures 8-11 The data in Tables 1 and 2 show that improper atmosphere control in the reactor leads to large liquid surface vortices, resulting in severe oxidation of the slurry inside the reactor and an increase in the specific surface area of ​​the precursor. Figures 8-11 The comparison of primary particles shows that if the atmosphere of the reactor is not properly controlled, the liquid surface vortex is large, which causes severe oxidation of the slurry in the reactor. This leads to the refinement of the primary particle whiskers of the precursor, loose stacking, and increased porosity. Therefore, the anti-oxidation system of the ternary precursor reactor in this embodiment not only solves the problem of insufficient nitrogen and large liquid surface vortex in the current ternary precursor reactor, which leads to oxidation of the ternary precursor, but also solves the problem of excessive nitrogen causing waste, saving a certain amount of nitrogen usage and reducing production costs.

[0080] In summary, the ternary precursor reactor anti-oxidation system disclosed in this application has the following advantages and positive effects:

[0081] 1. This invention utilizes an atmosphere analysis system 12 and an automated control system 14 to measure and automatically control the atmosphere containing ammonia, ensuring that the atmosphere inside the reactor remains at a high nitrogen concentration for an extended period. Simultaneously, the high nitrogen concentration in the reactor prevents the slurry produced from the reaction from being oxidized, thus improving product quality and reducing production risk costs. Furthermore, it effectively reduces labor costs.

[0082] 2. This utility model utilizes a vortex breaker 3 to reduce the problem of large vortices on the surface of the liquid in the reactor caused by increased stirring intensity, which makes the slurry in the reactor prone to oxidation, thereby improving the quality of the product.

[0083] 3. This utility model utilizes a gas mixer 4 to enable the nitrogen gas entering the reactor to be quickly and evenly mixed, reducing local oxidation caused by high local oxygen concentration. At the same time, it reduces the error in sampling and measurement due to uneven atmosphere, ensuring the accuracy of monitoring and reducing the frequent adjustment and consumption of nitrogen gas.

[0084] The embodiments of the present utility model have been described in detail above with reference to the accompanying drawings. However, the present utility model is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the spirit of the present utility model.

Claims

1. An anti-oxidation system for a ternary precursor reactor, characterized in that, include: The reactor body (1) is connected to an air inlet pipe (16), which is connected to an inert gas. The air inlet pipe (16) is equipped with a regulating valve (15) for adjusting the air intake of the inert gas. The reactor body (1) is equipped with a stirrer (2) for stirring the internal liquid. An atmosphere analysis system (12) is connected to a gas sampling tube (8). The gas sampling tube (8) is sequentially equipped with a vacuum pump (10) and a switching valve (5), and is ultimately connected to the reactor body (1). The atmosphere analysis system (12) can control the start and stop of the vacuum pump (10) and the switching valve (5). The atmosphere analysis system (12) is used to monitor the content of the inert gas in the reactor body (1) and generate gas content information. The control system (14) is used to acquire the gas content information and adjust the opening degree of the regulating valve (15) according to preset conditions.

2. The anti-oxidation system for a ternary precursor reactor according to claim 1, characterized in that: It also includes a vortex breaker (3), which includes a support frame (31) installed inside the reactor body (1) and a vortex-breaking plate (32) installed on the support frame (31). The vortex-breaking plate is inserted into the liquid surface of the internal liquid and is used to impede the vortex motion of the liquid surface.

3. The anti-oxidation system for a ternary precursor reactor according to claim 2, characterized in that: The number of the vortex breakers (3) is multiple, and the multiple vortex breakers (3) are arranged in a ring around the stirring center line of the stirrer (2).

4. The anti-oxidation system for a ternary precursor reactor according to claim 2, characterized in that: A rotating shaft and a limiting member are installed between the support frame (31) and the vortex-breaking plate (32). The length direction of the rotating shaft is parallel to the stirring center line of the stirrer (2). The vortex-breaking plate (32) can rotate relative to the support frame (31) around the rotating shaft to adjust the angle position of the vortex-breaking plate (32). The limiting member is used to fix the angle position of the vortex-breaking plate (32) after adjustment.

5. The anti-oxidation system for a ternary precursor reactor according to claim 4, characterized in that: The rotating shaft is a fixed rod (33) that passes through the support frame (31) and the vortex-breaking plate (32). The limiting member is a fixed nut (34). The fixed nut is threadedly connected to the fixed rod (33). When the fixed nut (34) is screwed in, the fixed nut (34) and the fixed rod (33) can clamp the support frame (31) and the vortex-breaking plate (32) to limit the rotation of the vortex-breaking plate (32) relative to the support frame (31).

6. The anti-oxidation system for a ternary precursor reactor according to claim 1 or 2, characterized in that: It also includes a gas mixer (4) installed at the top inside the reactor body (1). The gas mixer (4) is provided with a main air inlet (41) connected to the air inlet pipe (16) and an annular channel connected to the main air inlet (41). Multiple branch gas paths (42) are formed inside the gas mixer (4) and are arranged around the stirring center line of the stirrer (2). One end of the branch gas path (42) is a gas path inlet (43) connected to the annular channel, and the other end is a gas path outlet (44) connected to the inside of the reactor body (1).

7. The anti-oxidation system for a ternary precursor reactor according to claim 6, characterized in that: The direction of the line connecting the two ends of the multiple diversion gas paths (42) forms an angle β greater than 0 and less than 90 degrees with the circumferential radius direction of the annular channel, so that the diversion gas path (42) is inclined relative to the circumferential radius direction of the annular channel, and one end of the gas outlet (44) of the diversion gas path (42) is bent toward the stirring center line of the stirrer (2).

8. The anti-oxidation system for a ternary precursor reactor according to claim 6, characterized in that: The cross-sectional area of ​​the air inlet (43) is larger than the cross-sectional area of ​​the air outlet (44).

9. The anti-oxidation system for a ternary precursor reactor according to claim 1, characterized in that: The gas sampling tube (8) is also equipped with a dryer (7) and an ammonia absorber (9). The dryer (7) is located between the switch valve (5) and the pump (10), and the ammonia absorber (9) is located between the dryer (7) and the pump (10).

10. The anti-oxidation system for a ternary precursor reactor according to claim 9, characterized in that: The gas sampling tube (8) is also equipped with a first filter (6) and a second filter (11), the first filter (6) being located between the switching valve (5) and the dryer (7), and the second filter (11) being located between the air pump (10) and the atmosphere analysis system (12).

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