Continuous reaction system for preparing manganous-manganic oxide

Abstract

The utility model discloses a continuous reaction system for preparing manganous-manganic oxide. The continuous reaction system comprises a reaction kettle, a stirring device and a filtering device, a feeding pipe and an air inlet pipe are arranged on a top cover of the reaction kettle, a discharging pipe is arranged at the bottom of the reaction kettle, an overflow port is formed in the side wall of the reaction kettle, the overflow port is communicated with a feeding port of the stirring device through an overflow pipe, and a discharging port of the stirring device is communicated with a feeding port of the filtering device through a discharging and conveying mechanism. The system can realize efficient production of manganous-manganic oxide by a one-step method through the specially designed reaction kettle matched with the stirring device and the filtering device, and has the characteristic of continuous production, the obtained product has better quality, the product quality is relatively stable, and the production input cost is lower. In addition, the device has the advantages of simple structure, low equipment investment cost, convenience in operation, high production efficiency, stable production effect, high practicability and the like.

Description

Technical Field

[0001] This utility model relates to the preparation of battery materials, specifically to a continuous reaction system for preparing manganese tetroxide, belonging to the field of manganese tetroxide production technology. Background Technology

[0002] In recent years, with the development of green industries such as new energy vehicles, lithium manganese oxide (LiMn2O4), as a cathode material for power lithium-ion batteries, has received increasing attention due to its advantages such as low price, good safety performance, and no environmental pollution. Currently, lithium manganese oxide production mainly uses electrolytic manganese dioxide as the manganese source, which is then solid-state sintered with lithium carbonate and corresponding additives. However, due to defects such as poor particle morphology in electrolytic manganese dioxide, the prepared lithium manganese oxide material suffers from problems such as low specific capacity, poor cycle performance, and poor high-temperature performance. Mn3O4 and LiMn2O4 have the same spinel structure. When preparing LiMn2O4 using Mn3O4, no drastic structural changes occur, resulting in a more stable material structure. The prepared LiMn2O4 exhibits superior electrochemical performance, with significant improvements in specific capacity, high-temperature performance, and cycle performance. Therefore, using Mn3O4 to replace electrolytic manganese dioxide in the production of LiMn2O4 is the current development trend.

[0003] The main methods for preparing Mn3O4 include calcination, reduction, oxidation, and manganese salt methods. Currently, the oxidation method using a suspension of metallic manganese powder is widely used. This method is relatively mature, but it has high production costs, low purity, and uneven particle size. In recent years, the manganese salt method has received widespread attention due to its advantages such as low raw material costs. It can be divided into one-step and two-step methods. The two-step manganese salt method for preparing Mn3O4 involves two steps: first, an alkaline precipitant is added to the manganese salt to obtain Mn(OH)2 precipitate; after filtration and washing, the Mn(OH)2 is slurried and oxidized to obtain Mn3O4 particles. The two-step oxidation method requires the use of inert gas protection throughout the Mn(OH)2 preparation stage, making the process relatively complex, and the morphology and particle size of the product are difficult to control, making continuous production impossible. In contrast, the one-step method does not require the prior preparation of Mn(OH)2, but directly oxidizes Mn. 2+ The method for obtaining Mn3O4 is short and has high production efficiency. However, the equipment used for the one-step production of manganese tetroxide in the existing technology is relatively simple, and there are problems such as low production efficiency, poor product quality, and inability to produce continuously, which greatly limits the development of the one-step production of manganese tetroxide. Utility Model Content

[0004] In view of the problems of low production efficiency, poor product quality, and inability to produce manganese tetroxide in the existing one-step process, this utility model provides a continuous reaction system for the preparation of manganese tetroxide. The system, through a specially designed reaction vessel, combined with a stirring device and a filtration device, can achieve efficient one-step production of manganese tetroxide, and has the characteristics of continuous production. The resulting product has better quality, relatively stable product quality, and lower production input cost.

[0005] To achieve the above-mentioned technical objectives, the technical solution adopted by this utility model is as follows:

[0006] A continuous reaction system for preparing manganese tetroxide includes a reactor, a stirring device, and a filtration device. A feed pipe and an air inlet pipe are provided on the top cover of the reactor, a discharge pipe is provided at the bottom of the reactor, and an overflow port is provided on the side wall of the reactor. The overflow port is connected to the feed inlet of the stirring device through the overflow pipe, and the discharge port of the stirring device is connected to the feed inlet of the filtration device through a discharge and conveying mechanism.

[0007] Preferably, the top cover of the reactor is provided with multiple feed pipes, the lower ends of which penetrate the top cover and extend downward into the inner cavity of the reactor. Preferably, the lower ends of the feed pipes extend downward to the middle or lower part of the inner cavity of the reactor.

[0008] Preferably, the top cover of the reactor is provided with multiple air inlet pipes, the lower ends of which penetrate the top cover and extend downward into the inner cavity of the reactor. Preferably, the lower ends of the air inlet pipes extend downward to the middle or lower part of the inner cavity of the reactor.

[0009] Preferably, at least one exhaust pipe with a gas valve is also provided on the top cover of the reactor.

[0010] Preferably, a rotating shaft is also provided inside the reactor cavity. The upper end of the rotating shaft extends upward through the top cover of the reactor and outward, while the lower end extends downward to the lower part of the reactor cavity, below the bottom ends of the feed pipe and the air inlet pipe. A rotating paddle is also provided on the shaft body below the bottom ends of the feed pipe and the air inlet pipe.

[0011] Preferably, multiple layers of rotating paddles are arranged from top to bottom on the shaft below the bottom ends of the feed pipe and the air inlet pipe. The rotating paddles in each layer rotate in the same or opposite directions, and their rotation speeds are the same or different. Preferably, any two adjacent layers of rotating paddles rotate in opposite directions. More preferably, any two adjacent layers of rotating paddles rotate at different speeds.

[0012] Preferably, the reactor has a tapered opening structure, and the discharge pipe is installed through the lowest point of this tapered opening structure. The lower end of the discharge pipe extends downward to the outside of the reactor, and a discharge valve is also installed on the pipe body outside the reactor.

[0013] Preferably, a heating and insulation layer is also provided on the wall of the reactor, the heating and insulation layer consisting of an insulation layer and an electric heater disposed within the insulation layer.

[0014] Preferably, the overflow port is located on the upper part of the reactor wall, and within the reactor wall, the overflow port extends downwards in a gradually sloping manner from the interior of the reactor to the outside. Preferably, multiple overflow ports are provided on the upper part of the reactor wall from top to bottom. Preferably, an internal thread is provided at the outlet end of the overflow port, and a sealing head is detachably connected via the internal thread.

[0015] Preferably, the system includes multiple reactors connected in series. Specifically, the overflow port of the first reactor is connected to the overflow inlet on the upper part of the wall of the second reactor via a first overflow pipe; the overflow port of the second reactor is connected to the overflow inlet on the upper part of the wall of the third reactor via a second overflow pipe, and so on, with the overflow port of the last reactor connected to the inlet of the stirring device via a last overflow pipe. Preferably, the height of the multiple reactors gradually decreases according to the direction of the overflow material.

[0016] Preferably, the stirring device includes a storage tank and a stirring mechanism. The stirring mechanism is located inside the storage tank. The upper part of the storage tank has a feed inlet connected to an overflow pipe, and the bottom of the storage tank has a discharge outlet connected to a discharge and conveying mechanism.

[0017] Preferably, the discharge and conveying mechanism includes a discharge pipe, a conveying pump, and a conveying pipe. The inlet end of the discharge pipe is connected to the discharge port of the storage tank, and its discharge end is connected to the inlet end of the conveying pipe via the conveying pump. The discharge end of the conveying pipe is connected to the inlet end of the filter device. A conveying valve is also provided on the conveying pipe.

[0018] As a preferred option, a pH detection probe is also installed inside the reactor.

[0019] As a preferred option, a particle size detection probe is also installed on the overflow pipe.

[0020] Preferably, the system also includes a control device, which is independently connected to the reaction vessel, stirring device, and filtration device, and adjusts and controls the operating status of the reaction vessel, stirring device, and filtration device. Preferably, the control device is a PLC control cabinet.

[0021] In this invention, the continuous reaction system for preparing manganese tetroxide mainly comprises a reaction vessel (i.e., a reaction kettle), a stirring device, a filtration device, and detection elements (mainly used to detect various reaction parameters of the system during the reaction process). The reaction kettle has a relatively closed reaction chamber and is simultaneously connected to feeding, gas inlet, discharge, and overflow mechanisms, enabling the one-step preparation of manganese tetroxide within the reaction kettle. Furthermore, the overflow discharge design allows for a simultaneous feeding, reaction, and discharge production mode, achieving continuous production of manganese tetroxide and significantly improving production efficiency. Additionally, a control device may be included to achieve intelligent automatic production adjustment and control of the entire production system (mainly used to adjust and control various production parameters of the system), thereby reducing labor intensity and helping to ensure product quality stability.

[0022] In this invention, the reactor body is made of stainless steel or similar material, with an elliptical bottom (wider at the top and narrower at the bottom). A lid (made of stainless steel) is installed at the top of the reactor, with multiple round holes for accommodating a feed pipe and a gas inlet pipe (both made of stainless steel or Hastelloy, etc.). The feed pipe is used to add liquid materials to the reactor, and the gas inlet pipe is used to introduce one or more of nitrogen, oxygen, air, and argon into the reaction apparatus. An exhaust pipe with a valve is also installed on the lid to maintain stable internal pressure. It should be noted that the lower ends of both the feed pipe and the gas inlet pipe extend downwards to the lower middle part of the reactor cavity, allowing the incoming materials and gases to directly enter the lower part of the reactor. This ensures that the reaction mixture has sufficient reaction time during its ascent before flowing out from the overflow port located at the top of the reactor. Simultaneously, the rising reaction liquid also acts as a liquid seal for the feed pipe and the gas inlet pipe.

[0023] In this invention, a rotary stirring mechanism is also provided inside the reactor, including a rotating shaft and a rotary paddle (made of stainless steel or Hastelloy, etc.). The rotating shaft is vertically arranged, with its upper end passing through the top cover of the reactor and connected to an external motor. Its lower end is located inside the reactor and below the lowest points of the feed pipe and the air inlet pipe. A stirring paddle is designed on the shaft below the lowest points of the feed pipe and the air inlet pipe. The rotary stirring mechanism helps to quickly mix and react various reactants inside the reactor, improving reaction efficiency.

[0024] Furthermore, to improve the mixing efficiency of the reaction liquid, the stirring paddle is generally provided with multiple layers (all located below the lowest end of the feed pipe and the air inlet pipe), and the rotating paddles of each layer rotate in the same or opposite directions (e.g., by adding different reversing gears between the rotating shaft and the rotating paddle to make the rotating directions of different rotating paddles opposite), and their rotation speeds are the same or different (e.g., by setting different gear ratios between the rotating shaft and the rotating paddle to achieve differential rotation of different rotating paddles).

[0025] In this invention, a heating and insulation layer is also provided on the wall of the reactor. The heating method includes, but is not limited to, water bath, oil bath or electric heating, and is preferably a resistance heating device.

[0026] In this invention, the overflow port is located on the upper part of the reactor wall, and extends downwards in a gradually sloping manner from the inside of the reactor to the outside. Multiple overflow ports can be designed, and each overflow port has an internal thread at its outlet end. When an overflow port is not in use, it can be sealed with a plug (such as a plugging bolt) (or, if there is no thread, it can be sealed directly by plugging).

[0027] In this invention, the system includes multiple reaction vessels connected in series via overflow ports and overflow pipes. Each reaction vessel can also be individually fed with material and gas. To facilitate the smooth transfer of overflowing material, the height of the reaction vessels gradually decreases according to the direction of the overflowing material. It should be noted that this system is a continuous reaction device. During the reaction, materials can be added to each reaction vessel through the feed pipe, and the reaction atmosphere can be adjusted through the gas inlet pipe, introducing one or more of the required gases such as oxygen, nitrogen, and air into each reaction vessel to maintain the atmosphere inside each vessel. The bottom outlets of the liquid inlet pipe and gas inlet pipe are located near the tip of the upper blades of the agitator to ensure rapid dispersion of the material and gas within the reaction vessel, guaranteeing uniformity of the reaction system's composition and concentration, and improving gas-liquid contact to accelerate mass transfer.

[0028] In this invention, taking three reactors connected in series as an example, in the initial stage of the reaction, the materials are added in a certain order. The materials are first added to the first reactor through its feed pipe. During the feeding process, the liquid level continuously rises. When the liquid level reaches the overflow port of the first reactor, it flows out through the unsealed overflow port and then flows into the second reactor through the overflow pipe and the overflow inlet of the second reactor. At this point, materials can be added to the second reactor through its feed pipe. During the feeding process, the liquid level in the second reactor continuously rises. When the liquid level reaches the overflow port of the second reactor, it flows out through the unsealed overflow port and then flows into the third reactor through the overflow pipe and the overflow inlet of the third reactor. At this point, materials can be added to the third reactor through its feed pipe. During the feeding process, the liquid level in the third reactor continuously rises. When the liquid level reaches the overflow port of the third reactor, it flows out through the unsealed overflow port and then flows to the filtration device through the overflow channel. This involves using multiple reactors connected in series to achieve continuous production of battery-grade manganese tetroxide via wet processing, adapting to one-step preparation methods and increasing production efficiency.

[0029] In this invention, the stirring device includes a storage tank and a stirring device. The storage tank serves as a material buffer, and the stirring device prevents the solid components in the slurry from settling in the storage tank. Once the slurry level in the storage tank reaches a certain height, the discharge valve and the conveying valve can be opened, and the slurry can be conveyed to the filtration equipment by the conveying pump for solid-liquid separation to obtain the solid product.

[0030] In this invention, a pH detection probe is installed inside the reactor. A particle size detection probe is installed on the overflow pipe. The pH and particle size detection probes transmit the detected signals to the control device via signal lines, thereby feeding back real-time information on pH and particle size from the reactor and overflow pipe to the control device. The pH of the slurry is a crucial production parameter in the preparation of battery-grade manganese tetroxide, affecting the product phase and reaction rate; therefore, controlling the appropriate pH during the reaction is particularly important. Particle size is also a key product indicator for battery-grade manganese tetroxide; therefore, detecting the particle size of the product during the reaction and adjusting production parameters promptly based on the particle size information is of great significance for increasing product qualification rate and production efficiency.

[0031] In this invention, the control device includes a control cabinet and signal lines. The control cabinet is connected to the reactor, stirring device, and filtration device via the signal lines. More specifically, the control cabinet controls the start / stop of the heating and insulation device (i.e., the heating and insulation layer) of the reactor, the temperature inside the reactor, the start / stop of the stirring device, the stirring speed, the start / stop and flow regulation of the liquid inlet pipe, and the start / stop and flow regulation of the air inlet pipe, etc., via the signal lines; it also controls the start / stop of the stirring device, the stirring speed, the start / stop of the feed pump, and the start / stop of the filtration device in the storage tank; and it controls the start / stop of the detection equipment (pH detection probe and particle size detection probe) and signal transmission. It should be noted that when there are multiple reactors, the control device can individually control the start / stop of the heating and insulation device, the temperature inside the reactor, the start / stop of the stirring device, the stirring speed, the start / stop and flow regulation of the liquid inlet pipe, and the start / stop and flow regulation of the air inlet pipe, etc., in each reactor.

[0032] In this invention, all parts of the system are integrated into an organic whole through wiring and piping. Real-time monitoring parameters during the reaction process in the reactor can be fed back to the control device. When parameter adjustments are required, the control device can feed the adjustment information back to the reaction device, thereby achieving intelligent and automated control of the reactor system.

[0033] Compared with the prior art, the beneficial technical effects of this utility model are as follows:

[0034] 1. This utility model, through a specially designed reaction vessel, combined with a stirring device and a filtration device, can achieve efficient one-step production of manganese tetroxide, and has the characteristics of continuous production. The resulting product has better quality, relatively stable quality, and lower production input cost.

[0035] 2: This utility model can transmit and provide feedback on real-time pH and particle size information during the reaction process through a detection probe, thereby achieving stable production through real-time adjustment of process parameters and improving the automation and intelligence of the production process.

[0036] 3: The system of this utility model also has the advantages of simple structure, low equipment investment cost, convenient operation, high production efficiency, stable production effect and strong practicality. Attached Figure Description

[0037] Figure 1 This is a schematic diagram of the system described in this utility model.

[0038] Figure 2 This is a schematic diagram of the structure of the system described in this utility model when it has multiple reaction vessels.

[0039] Figure reference numerals: 1: Reactor; 101: Feed pipe; 102: Air inlet pipe; 103: Discharge pipe; 104: Overflow port; 105: Overflow pipe; 106: Exhaust pipe; 107: Rotating shaft; 108: Rotating paddle; 109: Discharge valve; 110: Heating and insulation layer; 111: Sealing head; 112: Overflow feed port; 113: pH detection probe; 114: Particle size detection probe; 2: Stirring device; 201: Storage tank; 202: Stirring mechanism; 203: Discharge and conveying mechanism; 3: Filtration device; 4: Control device. Detailed Implementation

[0040] The technical solution of this utility model is illustrated below. The scope of protection of this utility model includes, but is not limited to, the following embodiments.

[0041] A continuous reaction system for preparing manganese tetroxide includes a reactor 1, a stirring device 2, and a filtration device 3. A feed pipe 101 and an air inlet pipe 102 are provided on the top cover of the reactor 1, a discharge pipe 103 is provided at the bottom of the reactor, and an overflow port 104 is provided on the side wall of the reactor 1. The overflow port 104 is connected to the feed port of the stirring device 2 via an overflow pipe 105, and the discharge port of the stirring device 2 is connected to the feed port of the filtration device 3 via a discharge and conveying mechanism 203.

[0042] Preferably, a plurality of feed pipes 101 are provided on the top cover of the reactor 1, and the lower ends of the plurality of feed pipes 101 penetrate the top cover and extend downward into the inner cavity of the reactor 1. Preferably, the lower ends of the feed pipes 101 extend downward to the middle or lower part of the inner cavity of the reactor 1.

[0043] Preferably, a plurality of air inlet pipes 102 are provided on the top cover of the reactor 1, and the lower ends of the plurality of air inlet pipes 102 extend downward into the inner cavity of the reactor 1 after passing through the top cover. Preferably, the lower ends of the air inlet pipes 102 extend downward to the middle or lower part of the inner cavity of the reactor 1.

[0044] Preferably, at least one exhaust pipe 106 with a gas valve is also provided on the top cover of the reactor 1.

[0045] Preferably, a rotating shaft 107 is also provided in the inner cavity of the reactor 1. The upper end of the rotating shaft 107 extends upward through the top cover of the reactor 1 and outwards, while the lower end of the rotating shaft 107 extends downward to the lower part of the inner cavity of the reactor 1, below the bottom end of the feed pipe 101 and the bottom end of the air inlet pipe 102. A rotating paddle 108 is also provided on the shaft of the rotating shaft 107 below the bottom ends of the feed pipe 101 and the air inlet pipe 102.

[0046] Preferably, multiple layers of rotating paddles 108 are arranged from top to bottom on the shaft of the rotating shaft 107, below the bottom ends of the feed pipe 101 and the air inlet pipe 102. The rotation directions of each of the multiple layers of rotating paddles 108 are the same or opposite, and their rotation speeds are the same or different. Preferably, the rotation directions of any two adjacent layers of rotating paddles 108 are opposite. More preferably, the rotation speeds of any two adjacent layers of rotating paddles 108 are different.

[0047] Preferably, the reactor 1 has a tapered opening structure, and the discharge pipe 103 is disposed through the lowest point of the tapered opening structure. The lower end of the discharge pipe 103 extends downward to the outside of the reactor 1, and a discharge valve 109 is also provided on the pipe body of the discharge pipe 103 located outside the reactor 1.

[0048] Preferably, a heating and insulation layer 110 is also provided on the wall of the reactor 1, the heating and insulation layer 110 consisting of an insulation layer and an electric heater disposed within the insulation layer.

[0049] Preferably, the overflow port 104 is located on the upper part of the reactor 1 wall, and within the reactor 1 wall, the overflow port 104 extends downwards in a gradually sloping manner from the interior to the exterior of the reactor 1. Preferably, multiple overflow ports 104 are provided on the upper part of the reactor 1 wall from top to bottom. Preferably, an internal thread is provided at the outlet end of the overflow port 104, and a sealing head 111 is detachably connected via the internal thread.

[0050] Preferably, the system includes multiple reactors 1 connected in series. Specifically, the overflow port 104 of the first reactor 1 is connected to the overflow inlet 112 on the upper part of the wall of the second reactor 1 via a first overflow pipe 105; the overflow port 104 of the second reactor 1 is connected to the overflow inlet 112 on the upper part of the wall of the third reactor 1 via a second overflow pipe 105, and so on, until the overflow port 104 of the last reactor 1 is connected to the inlet of the stirring device 2 via a last overflow pipe 105. Preferably, the height of the multiple reactors 1 gradually decreases according to the direction of the overflow material.

[0051] Preferably, the stirring device 2 includes a storage tank 201 and a stirring mechanism 202. The stirring mechanism 202 is disposed inside the storage tank 201. The storage tank 201 has an inlet at the top connected to an overflow pipe 105 and a discharge port at the bottom connected to a discharge and conveying mechanism 203.

[0052] Preferably, the discharge and conveying mechanism 203 includes a discharge pipe, a conveying pump, and a conveying pipe. The inlet end of the discharge pipe is connected to the discharge port of the storage tank 201, and its discharge end is connected to the inlet end of the conveying pipe through the conveying pump. The discharge end of the conveying pipe is connected to the inlet end of the filter device 3. A conveying valve is also provided on the conveying pipe.

[0053] Preferably, a pH detection probe 113 is also installed inside the reaction vessel 1.

[0054] As a preferred option, a particle size detection probe 114 is also provided on the overflow pipe 105.

[0055] Preferably, the system also includes a control device 4, which is independently connected to the reaction vessel 1, the stirring device 2, and the filtering device 3. The control device 4 regulates and controls the operating status of the reaction vessel 1, the stirring device 2, and the filtering device 3. Preferably, the control device 4 is a PLC control cabinet. Example 1

[0056] like Figure 1-2 As shown, a continuous reaction system for preparing manganese tetroxide includes a reactor 1, a stirring device 2, and a filtration device 3. A feed pipe 101 and an air inlet pipe 102 are provided on the top cover of the reactor 1, a discharge pipe 103 is provided at the bottom of the reactor, and an overflow port 104 is provided on the side wall of the reactor 1. The overflow port 104 is connected to the feed port of the stirring device 2 via an overflow pipe 105, and the discharge port of the stirring device 2 is connected to the feed port of the filtration device 3 via a discharge and conveying mechanism 203. Example 2

[0057] Repeat Example 1, except that multiple feed pipes 101 are provided on the top cover of the reactor 1, and the lower ends of the multiple feed pipes 101 penetrate the top cover and extend downward into the inner cavity of the reactor 1. Example 3

[0058] Repeat Example 2, except that the lower end of the feed pipe 101 extends downward to the lower part of the inner cavity of the reactor 1. Example 4

[0059] Repeat Example 3, except that multiple air inlet pipes 102 are provided on the top cover of the reactor 1, and the lower ends of the multiple air inlet pipes 102 penetrate the top cover and extend downward into the inner cavity of the reactor 1. Example 5

[0060] Repeat Example 4, except that the lower end of the air inlet pipe 102 extends downward to the lower part of the inner cavity of the reactor 1. Example 6

[0061] Repeat Example 5, except that at least one exhaust pipe 106 with a gas valve is also provided on the top cover of the reactor 1. Example 7

[0062] The embodiment 6 is repeated, except that a rotating shaft 107 is also provided in the inner cavity of the reactor 1. The upper end of the rotating shaft 107 extends upward through the top cover of the reactor 1 and outward, while the lower end of the rotating shaft 107 extends downward to the lower part of the inner cavity of the reactor 1 and is lower than the bottom end of the feed pipe 101 and the bottom end of the air inlet pipe 102. A rotating paddle 108 is also provided on the shaft of the rotating shaft 107 below the bottom ends of the feed pipe 101 and the air inlet pipe 102. Example 8

[0063] Example 7 is repeated, except that multiple layers of rotating paddles 108 are arranged from top to bottom on the shaft of the rotating shaft 107, which is below the bottom ends of the feed pipe 101 and the air inlet pipe 102. The rotation directions of the multiple layers of rotating paddles 108 are the same or opposite, and their rotation speeds are the same or different. Example 9

[0064] Repeat Example 8, except that the rotation directions of any two adjacent rotating propellers 108 are opposite. Example 10

[0065] Example 9 is repeated, except that the rotational speeds of any two adjacent rotating propellers 108 are different. Example 11

[0066] Example 10 is repeated, except that the reactor 1 has a tapered opening structure, and the discharge pipe 103 is installed through the lowest point of the tapered opening structure. The lower end of the discharge pipe 103 extends downward to the outside of the reactor 1, and a discharge valve 109 is also provided on the pipe body of the discharge pipe 103 located outside the reactor 1. Example 12

[0067] The embodiment 11 is repeated, except that a heating and insulation layer 110 is also provided on the wall of the reactor 1. The heating and insulation layer 110 consists of an insulation layer and an electric heater disposed within the insulation layer. Example 13

[0068] Repeat Example 12, except that the overflow port 104 is opened on the upper part of the wall of the reactor 1, and the overflow port 104 extends downward in a gradually inclined manner along the direction from the inside of the reactor 1 to the outside. Example 14

[0069] Repeat Example 12, except that the upper part of the reactor 1 wall is provided with multiple overflow ports 104 from top to bottom. Example 15

[0070] The embodiment 14 is repeated, except that an internal thread is provided at the outlet end of the overflow port 104, and a plug head 111 is detachably connected through the internal thread. Example 16

[0071] Repeat Example 15, except that the system includes multiple reactors 1 connected in series. Specifically, the overflow port 104 of the first reactor 1 is connected to the overflow inlet 112 on the upper part of the wall of the second reactor 1 through the first overflow pipe 105. The overflow port 104 of the second reactor 1 is connected to the overflow inlet 112 on the upper part of the wall of the third reactor 1 through the second overflow pipe 105, and so on. The overflow port 104 of the last reactor 1 is connected to the inlet of the stirring device 2 through the last overflow pipe 105. Example 17

[0072] Example 16 is repeated, except that the height of the plurality of reactors 1 is gradually reduced according to the direction of the overflow material. Example 18

[0073] The embodiment 17 is repeated, except that the stirring device 2 includes a storage tank 201 and a stirring mechanism 202. The stirring mechanism 202 is located inside the storage tank 201. The storage tank 201 has an inlet at the top connected to the overflow pipe 105, and a discharge port at the bottom connected to the discharge and conveying mechanism 203. Example 19

[0074] The same method applies to embodiment 18, except that the discharge and conveying mechanism 203 includes a discharge pipe, a conveying pump, and a conveying pipe. The inlet end of the discharge pipe is connected to the discharge port of the storage tank 201, and its discharge end is connected to the inlet end of the conveying pipe via the conveying pump. The discharge end of the conveying pipe is connected to the inlet end of the filter device 3. A conveying valve is also provided on the conveying pipe. Example 20

[0075] Example 19 is repeated, except that a pH detection probe 113 is also installed in the reactor 1. Example 21

[0076] Example 20 is repeated, except that a particle size detection probe 114 is also provided on the overflow pipe 105. Example 22

[0077] The system repeats Example 21, except that it also includes a control device 4. The control device 4 is independently connected to the reactor 1, the stirring device 2, and the filtering device 3. The operating status of the reactor 1, the stirring device 2, and the filtering device 3 is adjusted and controlled by the control device 4. The control device 4 is a PLC control cabinet.

[0078] When preparing manganese tetroxide using the system described in this invention, the reaction raw materials are fed and inhaled through the feed pipe 101 and the air inlet pipe 102. Under a given atmosphere, the materials react with the reaction vessel 1 under the action of the rotating shaft 107 and the rotating paddle 108. As the materials continuously enter, the liquid level of the reaction system gradually rises and overflows from the overflow port 104, passing through the overflow pipe 105 into the inner cavity of the stirring device 2, where the reaction continues under the stirring action of the stirring mechanism 202. After the reaction is completed, the resulting reaction mixture is discharged through the discharge and conveying mechanism 203 into the filtration device 3 for separation to obtain a solid product. During the reaction process, the reaction progress can also be monitored in real time by the control device 4, the pH detection probe 113, and the particle size detection probe 114, so as to adjust the system production parameters in real time.

Claims

1. A continuous reaction system for the preparation of trimanganese tetraoxide, characterized in that: The system comprises a reaction kettle (1), a stirring device (2) and a filtering device (3); a feeding pipe (101) and an air inlet pipe (102) are arranged on the top cover of the reaction kettle (1), a discharge pipe (103) is arranged at the bottom of the reaction kettle, an overflow port (104) is arranged on the side wall of the reaction kettle (1), the overflow port (104) is connected with the feeding port of the stirring device (2) through an overflow pipe (105), and the discharge port of the stirring device (2) is connected with the feeding port of the filtering device (3) through a discharging and feeding mechanism (203).

2. The system of claim 1, wherein: A plurality of feeding pipes (101) are arranged on the top cover of the reaction kettle (1), and the lower ends of the plurality of feeding pipes (101) extend into the inner cavity of the reaction kettle (1) after penetrating through the top cover; and / or A plurality of air inlet pipes (102) are arranged on the top cover of the reaction kettle (1), and the lower ends of the plurality of air inlet pipes (102) extend into the inner cavity of the reaction kettle (1) after penetrating through the top cover.

3. The system of claim 2, wherein: The lower end of the feeding pipe (101) extends to the middle or lower part of the inner cavity of the reaction kettle (1); and the lower end of the air inlet pipe (102) extends to the middle or lower part of the inner cavity of the reaction kettle (1).

4. The system of claim 2, wherein: At least one exhaust pipe (106) with an air valve is further arranged on the top cover of the reaction kettle (1).

5. The system of claim 4, wherein: A rotating shaft (107) is further arranged in the inner cavity of the reaction kettle (1), the upper end of the rotating shaft (107) extends to the outside after penetrating through the top cover of the reaction kettle (1), the lower end of the rotating shaft (107) extends to the lower part of the inner cavity of the reaction kettle (1) and is lower than the bottom end of the feeding pipe (101) and the bottom end of the air inlet pipe (102), and a rotating paddle (108) is further arranged on the shaft of the rotating shaft (107) which is lower than the bottom end of the feeding pipe (101) and the bottom end of the air inlet pipe (102).

6. The system of claim 5, wherein: A plurality of layers of rotating paddles (108) are arranged on the shaft of the rotating shaft (107) which is lower than the bottom end of the feeding pipe (101) and the bottom end of the air inlet pipe (102) from top to bottom; the rotating directions of the rotating paddles (108) in the plurality of layers are the same or opposite, and the rotating speeds of the rotating paddles (108) in the plurality of layers are the same or different.

7. The system of claim 6, wherein: The rotating directions of any two adjacent layers of rotating paddles (108) are opposite.

8. The system of claim 6, wherein: The rotating speeds of any two adjacent layers of rotating paddles (108) are different.

9. The system of any one of claims 1-8, wherein: The reaction kettle (1) has a tapered structure, the discharge pipe (103) is arranged at the lowest part of the tapered structure in a penetrating mode, the lower end of the discharge pipe (103) extends to the outside of the reaction kettle (1), and a discharge valve (109) is further arranged on the pipe body of the discharge pipe (103) which is located outside the reaction kettle (1).

10. The system of any one of claims 1-8, wherein: A heating and heat preservation layer (110) is further arranged on the wall of the reaction kettle (1), the heating and heat preservation layer (110) is composed of a heat preservation layer and an electric heater arranged in the heat preservation layer; and / or The overflow port (104) is arranged at the upper part of the wall of the reaction kettle (1), and in the wall of the reaction kettle (1), the overflow port (104) extends in a downwardly inclined manner along the direction from the inside of the reaction kettle (1) to the outside.

11. The system of claim 10, wherein: A plurality of overflow ports (104) are arranged at the upper part of the wall of the reaction kettle (1) from top to bottom.

12. The system of claim 11, wherein: The overflow port (104) is provided with an internal thread at an outlet end, and a plug (111) is detachably connected through the internal thread.

13. The system of any one of claims 1-8, wherein: The system comprises a plurality of reaction kettles (1), and the plurality of reaction kettles (1) are sequentially connected in series. Specifically, the overflow port (104) of the first reaction kettle (1) is connected in communication with the overflow inlet (112) on the upper portion of the wall of the second reaction kettle (1) through the first overflow pipe (105), the overflow port (104) of the second reaction kettle (1) is connected in communication with the overflow inlet (112) on the upper portion of the wall of the third reaction kettle (1) through the second overflow pipe (105), and the like, and the overflow port (104) of the last reaction kettle (1) is connected in communication with the inlet of the stirring device (2) through the last overflow pipe (105). According to the direction of the overflow material, the heights of the plurality of reaction kettles (1) are gradually reduced.

14. The system of any one of claims 1-8, wherein: The stirring device (2) comprises a liquid storage tank (201) and a stirring mechanism (202). The stirring mechanism (202) is arranged in the liquid storage tank (201). The liquid storage tank (201) is provided with an inlet connected with the overflow pipe (105) at the upper portion, and is provided with a discharge port connected with the discharging and conveying mechanism (203) at the bottom.

15. The system of claim 14, wherein: The discharging and conveying mechanism (203) comprises a discharging pipe, a conveying pump and a conveying pipe. The inlet end of the discharging pipe is connected with the discharge port of the liquid storage tank (201), the discharge end of the discharging pipe is connected with the inlet end of the conveying pipe through the conveying pump, and the discharge end of the conveying pipe is connected with the inlet end of the filtering device (3). A conveying valve is further arranged on the conveying pipe.

16. The system of any one of claims 1-8, wherein: A pH detection probe (113) is further arranged in the reaction kettle (1). A particle size detection probe (114) is further arranged on the overflow pipe (105).

17. The system of claim 16, wherein: The system further comprises a control device (4). The control device (4) is independently connected in signal with the reaction kettle (1), the stirring device (2) and the filtering device (3), and the working states of the reaction kettle (1), the stirring device (2) and the filtering device (3) are adjusted and controlled through the control device (4).

18. The system of claim 17, wherein: The control device (4) is a PLC control cabinet.

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