Trimanganese tetroxide synthesis kettle
By designing a trimanium tetraoxide synthesis kettle, and using the feedback control system to accurately control the reaction conditions and material residence time, the problem that existing oxidation equipment cannot accurately control the reaction is solved, and the efficient, precise control and automation of trimanium tetraoxide reaction is achieved.
Patent Information
- Application Number
- CN202421522912.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-01
- Publication Date
- 2025-06-10
- Estimated Expiration
- 2034-07-01
AI Technical Summary
The existing oxidation method to prepare trimanganese tetraoxide reaction equipment cannot accurately control the reaction conditions and the residence time of the reaction materials in the kettle body, which affects the reaction process and has low automation.
A trimanganese tetraoxide synthetic kettle was designed, including the kettle body, cover plate, metal coil, stirring device and control system. Through the feedback from the liquid level meter, pH meter and thermometer, the reaction conditions and material residence time were accurately controlled to achieve complete control of the reaction.
It realizes efficient and precise control of trimanganese tetraoxide reaction, improves the degree of automation, reduces costs, and can fully recycle and utilize the raw materials, and the reaction is free of pollutants.
Smart Images
Figure CN222956365U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of manganese tetraoxide production, and particularly relates to a manganese tetraoxide synthesis kettle. Background Technique
[0002] Manganese tetraoxide is an oxide, black tetragonal crystal, mainly used in the fields of soft magnetic materials, semiconductor electronic materials, battery materials and glass manufacturing. Among them, battery-grade manganese tetraoxide has the characteristics of high-temperature stability and environmental protection.
[0003] At present, the preparation of manganese tetraoxide in China mainly includes four categories: roasting method, reduction method, oxidation method and electrolysis method. The roasting method is to burn metal manganese or manganese oxides, hydroxides, sulfates, carbonates, sulfites, nitrates and permanganates in air or oxygen at 1000 °C, and then obtain manganese tetraoxide after cooling and crushing. The reduction method uses manganese dioxide or manganite as raw materials, first roasted into manganese sesquioxide, and then further reduced at 250-500 °C in a methane atmosphere to generate manganese tetraoxide, and the finished product of manganese tetraoxide is obtained after cooling and crushing. The manganese tetraoxide obtained by the electrolysis method can be obtained by heating in air at 1050 °C. Among them, due to the limitations of process conditions, cost raw materials, product quality and other factors, only a few enterprises have achieved industrialization for the roasting method, reduction method and electrolysis method.
[0004] The oxidation method is to add complexing agents such as ammonia / sodium hydroxide solution to the manganese sulfate / manganese chloride ion solution, control the reaction temperature at about 70 °C and introduce air, keep the pH value of the solution between 7 and 10, so that the manganese ions are converted into Mn(OH) 2 2 precipitate, and then air oxidation for 6-12 hours can obtain a manganese tetraoxide solution. The manganese tetraoxide solution is filtered and dried to obtain manganese tetraoxide crystals, and the solution can be reused. The reaction principle is as follows:
[0005] Mn 2+ 2+ +2(OH) - - →Mn(OH) 2 2
[0006] 3Mn(OH) 2 2 +O 2 2 →Mn 3 3 O 4 4 +2H 2 2 O 3 3 Mn(OH) 2 2 +O 2 2 →Mn 3 3 O 4 4 +2H 2 2 O
[0007] The existing reaction equipment for preparing manganese tetraoxide by oxidation method cannot precisely control the reaction conditions and the residence time of the reaction materials in the kettle body, thus affecting the reaction process, unable to achieve precise control of the reaction process, and having a low degree of automation. Utility Model Content
[0008] The problem to be solved by this utility model is to provide a manganese tetraoxide synthesis kettle in view of the deficiencies of the prior art, which has a simple structure, is easy to use, has a long service life, can effectively and precisely control the reaction conditions and the residence time of the reaction materials in the kettle body, and makes the reaction complete.
[0009] To achieve the above object, this utility model adopts the following technical solutions:
[0010] The described manganese tetraoxide synthesis kettle includes a kettle body, a cover plate, a metal coiled pipe, a stirring device and a control system. The kettle body is fixed to the cover plate by bolts. Longitudinal baffles are arranged on the inner wall of the kettle body, and mounting holes are provided on the baffles. An overflow port and a thermometer port are arranged on the side wall of the kettle body. A discharge port is arranged in the center of the bottom of the kettle body, and connection points are arranged around the bottom of the kettle body. The metal coiled pipe is arranged in the middle of the kettle body and fixed to the baffle and the connection points by bolts and clamps. The cover plate is arranged above the kettle body. A stirring port is arranged in the center of the cover plate, and a liquid inlet, a steam port, a pH meter port, a blast port, an exhaust port, a liquid level meter port, a manhole and a spare port are arranged at intervals on the circumference of the cover plate. A stirring device is arranged on the stirring port, and the stirring device extends through the stirring port into the interior of the kettle body. Sleeves are arranged on the liquid inlet and the blast port, leading directly to the bottom of the kettle body, and the sleeves are fixed to the connecting plate.
[0011] The described manganese tetraoxide synthesis kettle has a cylindrical structure for the kettle body, and the bottom of the kettle is in a conical or elliptical structure. The material is fiberglass, and support plates are evenly arranged on the outer side of the bottom of the kettle to bear the load during the operation of the synthesis kettle.
[0012] The described manganese tetraoxide synthesis kettle is provided with a lining layer on the inner side of the kettle body. The lining layer is a wear-resistant structural layer with wear-resistant characteristics and is a structure of epoxy vinyl ester resin plus silicon carbide.
[0013] The described manganese tetraoxide synthesis kettle is provided with an overflow port at a position 300 mm - 500 mm from the top of the kettle body, and the overflow port is connected with an overflow conduit leading to the bottom of the kettle.
[0014] The described manganese tetraoxide synthesis kettle is provided with a sampling port on the pipeline of the discharge port at the bottom of the kettle to sample and detect whether the product manganese tetraoxide meets the standards at irregular intervals.
[0015] The described manganese tetraoxide synthesis kettle, the liquid inlets provided on the cover plate include a first liquid inlet, a second liquid inlet, and a third liquid inlet. Among them, both the first liquid inlet and the second liquid inlet are multiple pipe orifices, and each type of liquid inlet is evenly distributed on the cover plate. The liquid inlets are all equipped with sleeves that lead directly to the bottom of the kettle, and the sleeves are all made of wear-resistant materials. The sleeves are fixed through the connecting plates provided on the kettle body.
[0016] The described manganese tetraoxide synthesis kettle, the metal coil pipe has a diameter of φ32 - φ57, is in a spiral structure, and the material is titanium.
[0017] The described manganese tetraoxide synthesis kettle, the stirring device is fixedly installed on the cover plate, and the lower end of the stirring device extends to the bottom of the kettle. The stirring operation speed is controlled at 135 - 145 Rad / min.
[0018] The described manganese tetraoxide synthesis kettle has a set of control systems. A radar level gauge is provided at the level gauge port, a feedback type thermometer is provided at the thermometer port, a Roots blower is connected to the air inlet, and the air volume is 120 Nm 3 / h. A feedback type pH meter is provided at the pH meter port. The radar level gauge, the feedback type thermometer, the Roots blower, and the feedback type pH meter are all electrically connected to the control system. After the above instruments are set by data, they perform interlocking feedback to achieve the automatic control of the system.
[0019] Compared with the prior art, the advantages of the present utility model are as follows: By the feedback of the liquid level data and pH data in the kettle, the inflow of manganese chloride solution and sodium hydroxide solution is controlled to maintain the reaction pH value at a specific value; By the data feedback of the thermometer, the amount of steam in the metal coil pipe is adjusted to maintain the reaction temperature at a specific value, ensuring the complete reaction of manganese tetraoxide. Compared with other reaction equipment for manganese tetraoxide, the present utility model has a simple structure, low equipment investment, less equipment maintenance, low cost, and can achieve a synthesis reaction with high efficiency and precise control.
[0020] The manganese tetraoxide obtained by the oxidation method using the synthesis kettle of the present utility model has an easily controllable process, the raw materials can be fully recycled, and no pollutants are generated during the reaction. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 It is a schematic structural diagram of the manganese tetraoxide synthesis kettle of the utility model;
[0022] Figure 2 It is a schematic diagram of the cover plate pipe orifices and the bottom structure of the manganese tetraoxide synthesis kettle of the present utility model;
[0023] In the figure: 1. Kettle body; 2. Cover plate; 3. Metal coil pipe; 4. Stirring device; 5. Control system; 1-1. Baffle plate; 1-2. Overflow port; 1-3. Thermometer port; 1-4. Discharge port; 1-5. Sampling port; 1-6. Support plate; 2-1. Stirring port; 2-2. Liquid inlet; 2-2a. First liquid inlet; 2-2b. Second liquid inlet; 2-2c. Third liquid inlet; 2-3. Steam port; 2-4. pH meter port; 2-5. Air inlet; 2-6. Exhaust port; 2-7. Liquid level gauge port; 2-8. Manhole. Specific embodiments
[0024] The following further describes the present utility model in conjunction with the accompanying drawings of the specification:
[0025] As Figure 1 - Figure 2 shown, a manganese tetraoxide synthesis kettle of the present utility model includes a kettle body 1, a cover plate 2, a metal coil pipe 3, a stirring device 4 and a control system 5. A baffle plate 1-1 is arranged on the inner wall of the kettle body 1, and an installation hole is provided on the baffle plate 1-1. An overflow port 1-2 and a thermometer port 1-3 are arranged on the side wall of the kettle body 1, and a discharge port 1-4 is arranged in the center of the bottom of the kettle body 1; the metal coil pipe 3 is fixed to the baffle plate 1-1 through bolts and clamps; a stirring port 2-1 is arranged at the center of the cover plate 2, and liquid inlets 2-2, a steam port 2-3, a pH meter port 2-4, an air inlet 2-5, an exhaust port 2-6, a liquid level gauge port 2-7 and a manhole 2-8 are arranged at intervals on the circumference of the cover plate 2; the stirring device 4 is arranged on the stirring port 2-1. A first liquid inlet 2-2a, a second liquid inlet 2-2b and a third liquid inlet 2-2c are arranged on the cover plate 2, wherein both the first liquid inlet 2-2a and the second liquid inlet 2-2b are multiple pipe orifices, and each type of liquid inlet 2-2 is evenly distributed on the cover plate 2. The liquid inlets 2-2 are all equipped with sleeves leading directly to the bottom of the kettle, and the sleeves are all made of wear-resistant materials and are fixed through a connecting plate arranged on the kettle body 1.
[0026] The process of the present utility model: In the above-mentioned manganese tetraoxide synthesis kettle, all pipe orifice valves are closed at the start of the process system. The valve is opened, and pure water is injected into the kettle body 1 through the third liquid inlet 2-2c. When the water injection liquid level reaches the 1 / 3 position of the kettle body 1, the feedback liquid level gauge on the liquid level gauge port 2-7 conducts data feedback to cut off the liquid inlet of the third liquid inlet 2-2c and start the stirring device 4 for stirring operation. The stirring speed is slowly increased and then stabilized at 140 rad / min. The first liquid inlet 2-2a and the second liquid inlet 2-2b are opened simultaneously, and a manganese chloride solution and a sodium hydroxide solution are respectively injected into the kettle. The flow rate of the manganese chloride solution is 0.6 m 3 / h; The pH meter on the pH meter port 2-4 monitors the pH data in the kettle body 1 in real time. Through the feedback of the pH meter, the injection amount of the sodium hydroxide solution is adjusted to maintain the pH in the kettle body 1 at about 10. At the same time, the steam valve is opened, and the steam enters the metal coil 3 through the steam port 2-3 to heat the mixed solution in the kettle body 1. The steam intake is adjusted through the feedback of the thermometer on the thermometer port 1-3 to maintain the reaction temperature at 70 °C. At this time, the Roots blower blows oxygen-containing air into the kettle body 1 through the air inlet 2-5 for the synthesis reaction. After that, as the reaction proceeds, the reaction solution is sampled and analyzed multiple times through the sampling port 1-5. When the particle size of the manganese tetroxide reaches the standard, the machine is stopped with one key, that is, the feeding of the manganese chloride solution, the sodium hydroxide solution, the steam, and the air is shut off. The valve on the bottom discharge port 1-4 of the kettle body 1 is opened, and the reaction solution in the kettle body 1 is emptied to collect the manganese tetroxide. The production operation of manganese tetroxide is carried out in such a cycle.
Claims
1. A manganese tetraoxide synthesis reactor, characterized in that: The synthesis kettle comprises a kettle body (1), a cover plate (2), a metal coil (3), a stirring device (4) and a control system (5); a baffle (1-1) is arranged on the inner wall of the kettle body (1), a mounting hole is arranged on the baffle (1-1), an overflow port (1-2) and a thermometer port (1-3) are arranged on the side wall of the kettle body (1), and a discharge port (1-4) is arranged in the middle of the bottom of the kettle body (1); the metal coil (3) is arranged in the middle of the kettle body (1) and is fixed to the baffle (1-1) by bolts and a clamp; A cover plate (2) is arranged above the kettle body (1); a stirring port (2-1) is arranged at the center of the cover plate (2); a liquid inlet (2-2), a steam port (2-3), a pH meter port (2-4), an air blast port (2-5), an exhaust port (2-6), a liquid level meter port (2-7), and a manhole (2-8) are arranged at intervals on the circumference of the cover plate (2); a stirring device (4) is arranged on the stirring port (2-1); the stirring device (4) passes through the stirring port (2-1) and extends into the interior of the kettle body (1).
2. The manganese tetraoxide synthesis reactor according to claim 1, characterized in that: The kettle body (1) is a cylindrical structure, the kettle bottom is a conical or elliptical structure, and the material is glass fiber reinforced plastic. Support plates (1-6) are evenly arranged on the outer side of the kettle bottom to bear the load when the synthesis kettle is in operation.
3. The manganese tetraoxide synthesis reactor according to claim 1, characterized in that: An inner lining layer is arranged on the inner side of the kettle body (1), and the inner lining layer is a wear-resistant structural layer having wear-resistant properties.
4. The manganese tetraoxide synthesis reactor according to claim 2, characterized in that: The overflow port (1-2) is arranged at a position 300 mm to 500 mm away from the top of the kettle body (1), and the overflow port (1-2) is connected to an overflow conduit leading to the bottom of the kettle.
5. The manganese tetraoxide synthesis reactor according to claim 2, characterized in that: A sampling port (1-5) is provided on the pipeline of the discharge port (1-4) at the bottom of the kettle, and is used for sampling at irregular intervals to detect whether the product manganese tetraoxide meets the standard.
6. The manganese tetraoxide synthesis reactor according to claim 1, characterized in that: The liquid inlets (2-2) provided on the cover plate (2) comprise a first liquid inlet (2-2a), a second liquid inlet (2-2b), and a third liquid inlet (2-2c), wherein the first liquid inlet (2-2a) and the second liquid inlet (2-2b) are both multiple pipe openings, and each type of liquid inlet (2-2) is distributed on the cover plate (2).
7. The trimanganese tetraoxide synthesis reactor according to claim 6, characterized in that: The liquid inlets (2-2) are all equipped with sleeves that pass directly through the bottom of the kettle. The sleeves are all made of wear-resistant materials and are fixed by connecting plates provided on the kettle body (1).
8. The manganese tetraoxide synthesis reactor according to claim 1, characterized in that: The diameter of the metal coil (3) is φ32-φ57 and has a spiral structure.
9. The manganese tetraoxide synthesis reactor according to claim 1, characterized in that: The stirring device (4) is fixedly mounted on the cover plate (2), and the lower end of the stirring device (4) extends to the bottom of the kettle.
10. The trimanganese tetraoxide synthesis reactor according to claim 1, characterized in that: It has a control system (5), a radar level gauge is provided at the level gauge port (2-7), a feedback type thermometer is provided at the thermometer port (1-3), and a Roots blower is connected to the air blast port (2-5), with an air volume of 120 Nm 3 / h, a feedback-type pH meter is provided at the pH meter port (2-4), and the radar level meter, feedback-type thermometer, Roots blower and feedback-type pH meter are all electrically connected to the control system (5) and perform interlocking feedback after data setting, thereby realizing automatic control of the system.