Battery-grade manganous-manganic oxide preparation system

Abstract

The utility model discloses a battery-grade manganous-manganic oxide preparation system which comprises a reaction kettle as well as a first storage tank, a second storage tank and a third storage tank which are connected with a feeding hole of the reaction kettle, the first storage tank is used for storing a slow-release agent, and a first feeding pump is arranged on a conveying pipe, connected with the reaction kettle, of the first storage tank; the second storage tank is used for storing a manganese sulfate solution; a second feeding pump is arranged on a conveying pipe for connecting the second storage tank and the reaction kettle; the third storage tank is used for storing alkali liquor, and a first feeding pump is arranged on a conveying pipe, connected with the reaction kettle, of the third storage tank; the reaction kettle is also connected with an oxidizing agent conveying pipe; a control valve is arranged on the oxidizing agent conveying pipe; a sampling port is formed in the reaction kettle and is connected with the particle size analyzer and the pH monitor respectively; a discharge hole is formed in the bottom of the reaction kettle. According to the utility model, the battery-grade manganous-manganic oxide product with higher purity and better performance can be obtained while the particle size is controlled.

Description

Technical Field

[0001] The utility model relates to the field of manganese tetraoxide preparation systems, in particular to a battery-grade manganese tetraoxide preparation system. Background Art

[0002] At present, the methods for producing battery-grade manganese tetraoxide in the industry mainly include metal manganese sheet oxidation method and manganese sulfate solution oxidation method. Among them, the metal manganese sheet oxidation method is to crush the electrolytic metal manganese sheet into a suspension and then use air oxidation to prepare manganese tetraoxide. This method has a simple process, high manganese recovery rate and large output, but the electrolytic metal manganese raw material is expensive, the obtained product has a low specific surface area, low activity, high Se content, and is easy to affect the environment. The manganese sulfate solution oxidation method is to add manganese sulfate solution and alkaline solution to the reactor at the same time to react to generate manganese hydroxide precipitation, and then use air to oxidize the manganese hydroxide precipitation into manganese tetraoxide; this scheme has the characteristics of high reaction rate and too fast particle growth in the actual preparation process, resulting in the easy encapsulation of impurities and too fast growth of the manganese tetraoxide product. It can also reduce the actual production efficiency. Therefore, the utility model aims to develop a battery-grade manganese tetraoxide preparation system to facilitate the batch production and control of battery-grade manganese tetraoxide, and to obtain higher-quality battery-grade manganese tetraoxide products, thereby promoting the further development and application of manganese tetraoxide as a high-quality manganese source for lithium manganate. Utility Model Content

[0003] The technical problem solved by the utility model is to provide a battery-grade manganese tetraoxide preparation system to solve the shortcomings of the above-mentioned background technology.

[0004] The technical problem solved by the utility model is achieved by the following technical solutions:

[0005] A battery-grade manganese tetraoxide preparation system comprises a reactor and a first storage tank, a second storage tank and a third storage tank connected to a feed port of the reactor; the first storage tank is used to store a slow-release agent, and a first feed pump is provided on a feed pipe connecting the first storage tank and the reactor; the second storage tank is used to store a manganese sulfate solution, and a second feed pump is provided on a feed pipe connecting the second storage tank and the reactor; the third storage tank is used to store an alkali solution, and a first feed pump is provided on a feed pipe connecting the third storage tank and the reactor; the reactor is also connected to an oxidant delivery pipe, and a control valve is provided on the oxidant delivery pipe; a sampling port is provided on the reactor, and the sampling port is respectively connected to a particle size analyzer and a pH monitor; a discharge port is provided at the bottom of the reactor.

[0006] In the utility model, a stirring structure is arranged in the reactor, and the stirring mechanism comprises multiple layers of stirring paddles, and the diameters of the blades of the multiple layers of stirring paddles decrease from top to bottom.

[0007] In the utility model, the stirring mechanism comprises three layers of stirring paddles, the blades of adjacent stirring paddles are staggered, and the ratio of the blade diameters of the stirring paddles from top to bottom is 2-2.5:1.2-1.8:1.

[0008] The utility model further comprises a controller, and the stirring mechanism, the particle size analyzer, the pH monitor, the first feed pump, the second feed pump, the third feed pump, and the control valve are all electrically connected to the controller.

[0009] The utility model also includes an alarm, which is electrically connected to the controller.

[0010] In the utility model, a temperature sensor is also arranged in the reactor, and the temperature sensor is electrically connected to the controller.

[0011] In the utility model, the discharge port of the reaction kettle is connected to the filtering device and the drying device in sequence.

[0012] Beneficial effects: The battery-grade manganese tetraoxide preparation system described in the utility model can control the growth rate of manganese tetraoxide particles by linking particle size monitoring and sustained-release agent feed amount during the reaction process, and maintain the pH of the reaction system by linking pH monitoring and alkali solution feed amount, thereby controlling the product particle size while improving the product purity.

[0013] The battery-grade manganese tetraoxide preparation system of the utility model can further enhance the dispersion of materials, refinement of droplets and reduce the resistance of stirring paddles through the improvement of the stirring mechanism, thereby effectively improving energy utilization efficiency and oxidation rate.

[0014] The battery-grade manganese tetraoxide preparation system described in the utility model uses a three-layer stirring paddle to ensure the uniform movement of the reaction materials, rather than being limited to a certain area. The length of the three-layer paddle blades decreases from top to bottom and is within a predetermined range, which can make the slurry flow in an ideal mixing state and effectively avoid the stirring "dead zone", so that the input energy is more effectively transferred to the reaction material system. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of a preferred embodiment of the utility model.

[0016] Figure 2 This is the control principle diagram of the utility model.

[0017] Figure 3 It is a structural schematic diagram of the stirring mechanism in the utility model.

[0018] Figure 4 This is a top view of the stirring mechanism in the present invention.

[0019] Among them: 1. Reactor; 2. First storage tank; 3. Second storage tank; 4. Third storage tank; 5. First feed pump; 6. Second feed pump; 7. Third feed pump; 8. Particle size analyzer; 9. pH monitor; 10. Oxidant delivery pipe; 11. Stirring mechanism; 12. Controller; 13. Temperature sensor; 14. Alarm. DETAILED DESCRIPTION

[0020] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further described below with reference to specific illustrations.

[0021] See also Figure 1 A battery-grade manganese tetraoxide preparation system shown includes a reactor 1 and a first storage tank 2, a second storage tank 3 and a third storage tank 4 connected to a feed port of the reactor 1.

[0022] The first storage tank 2 is used to store a slow-release agent, which is one or more of EDTA, sodium acetate, sodium oxalate and sodium tartrate; a first feed pump 5 is provided on the feed pipe connecting the first storage tank 2 and the reactor 1; the second storage tank 3 is used to store manganese sulfate solution, and a second feed pump 6 is provided on the feed pipe connecting the second storage tank 3 and the reactor 1; the third storage tank 4 is used to store alkali solution, and a first feed pump 5 is provided on the feed pipe connecting the third storage tank 4 and the reactor 1; the reactor 1 is also connected to an oxidant delivery pipe 10, and a control valve is provided on the oxidant delivery pipe 10; the oxidant is preferably one or more of air, oxygen and hydrogen peroxide. When the oxidant is air or oxygen, the oxidant delivery pipe 10 is a gas delivery pipe, and when the oxidant is hydrogen peroxide, the oxidant delivery pipe 10 is a liquid delivery pipe. Figure 1 As shown, the reactor 1 is provided with a sampling port. In this embodiment, the sampling port is an automatic sampling port provided at the lower part of the reactor 1. A control valve is provided at the sampling port to realize regular or irregular automatic sampling. The sampling port is connected to the particle size analyzer 8 and the pH monitor 9 through a sample delivery tube, respectively, so that the sample automatically enters the particle size analyzer 8 for particle size monitoring and automatically enters the pH monitor 9 for pH value testing. During the reaction process, the particles in the blades are regularly monitored by the particle size analyzer 8. When the growth rate of the particles is detected to be too fast, the feed amount of the sustained-release agent is increased by the first feed pump 5. When the growth rate of the detected particles is too slow, the feed amount of the sustained-release agent is reduced by the first feed pump 5, thereby preventing the particle size from growing too fast and causing a loose structure, or from growing too slowly and causing impurities to co-precipitate and affect the product purity and production efficiency. When the established particle size requirement is reached, the feed can be stopped in time to make the product better meet the actual needs. Furthermore, during the production process, the reaction pH of the system is maintained within a predetermined range through the linkage control of the pH monitor 9 and the first feed pump 5, which is beneficial to promoting the smooth progress of the reaction and obtaining a product with high purity and few impurities.

[0023] A discharge port is provided at the bottom of the reactor 1, and the liquid after the reaction in the reactor 1 is discharged from the discharge port. In a preferred embodiment, the discharge port of the reactor 1 is connected to a filtering device and a drying device in sequence, so that the liquid after the reaction is filtered and then dried to obtain a battery-grade manganese tetraoxide product.

[0024] As an improvement to this embodiment, Figure 1 As shown, the reactor 1 is provided with a stirring structure, and the stirring mechanism 11 includes multiple layers of stirring paddles, and the diameters of the blades of the multiple layers of stirring paddles decrease from top to bottom. This can further enhance the dispersion of the materials in the reactor 1, refine the droplets, and reduce the resistance of the stirring paddles, effectively improving the energy efficiency and oxidation rate. In a further improved embodiment, as Figure 3 and Figure 4 As shown, the stirring mechanism 11 includes three layers of stirring paddles, the blades of adjacent stirring paddles are staggered, and the ratio of the blade diameters of the stirring paddles from top to bottom is 2 to 2.5:1.2 to 1.8:1. The use of three layers of stirring paddles can ensure the uniform movement of the reaction materials, rather than being limited to movement in a certain area. The length of the three-layer paddle blades decreases from top to bottom and is within a predetermined range, which can make the slurry flow in an ideal mixing state, and can effectively avoid the stirring "dead zone", so that the input energy is more effectively transferred to the reaction material system, which is conducive to further ensuring the uniformity of the reaction and improving the overall quality of the product.

[0025] In order to further improve the intelligence level of the utility model, as an improvement to the present embodiment, a controller 12 is further included, such as Figure 2 As shown, the stirring mechanism 11, the particle size analyzer 8, the pH monitor 9, the first feed pump 5, the second feed pump 6, the third feed pump 7, and the control valve are all electrically connected to the controller 12. Therefore, in actual production, the first feed pump 5, the second feed pump 6, the third feed pump 7, and the control valve can be adjusted according to the data detected by the particle size analyzer 8 and the pH monitor 9, and the feed amount of each raw material can be further adjusted to achieve dynamic adjustment. The stirring mechanism 11 is electrically connected to the controller 12, and the stirring rate can be adjusted according to the different requirements of the particle nucleation, growth and aging stages, thereby improving the sphericity of the manganese tetraoxide particles.

[0026] As an improvement to this embodiment, an alarm 14 is further included, and the alarm 14 is electrically connected to the controller 12. When the product particle size meets the requirements and the reaction is completed, the alarm 14 sounds to prompt the operator to perform further operations.

[0027] In the present invention, the reaction is carried out at a temperature of 50 to 70° C. To better meet the production requirements, a temperature sensor 13 is further provided in the reactor 1 , and the temperature sensor 13 is electrically connected to the controller 12 .

[0028] The system described in the utility model can produce manganese tetraoxide products with controllable particle size, good product consistency, good spherical shape, compact structure, few impurities and high purity. According to the test, the particle size of the manganese tetraoxide product obtained by the system described in the utility model is 6.04μm, the Mn content is more than 71%, the S content is 0.06%, and the tap density is 2.20g / cm3; while as a traditional non-linkage control preparation system, the particle size of the manganese tetraoxide product obtained is 6.26μm, the Mn content is 68.73%, the S content is 0.25%, and the tap density is 1.55g / cm 3 This shows that the utility model has better practical promotion and application prospects.

[0029] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0030] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the present utility model, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0031] In the present utility model, unless otherwise clearly stipulated and limited, the terms such as "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, or it can be the internal connection of two elements.

[0032] The above contents are further detailed descriptions of the present invention in combination with specific implementation methods, and it cannot be determined that the specific implementation of the present invention is limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, several simple deductions or substitutions can be made without departing from the concept of the present invention.

Claims

1. A battery-grade manganese tetraoxide preparation system, characterized in that: The invention comprises a reactor and a first storage tank, a second storage tank and a third storage tank connected to a feed port of the reactor; the first storage tank is used to store a slow-release agent, and a first feed pump is arranged on a feed pipe connecting the first storage tank and the reactor; the second storage tank is used to store a manganese sulfate solution, and a second feed pump is arranged on a feed pipe connecting the second storage tank and the reactor; the third storage tank is used to store an alkali solution, and a first feed pump is arranged on a feed pipe connecting the third storage tank and the reactor; the reactor is also connected to an oxidant delivery pipe, and a control valve is arranged on the oxidant delivery pipe; a sampling port is arranged on the reactor, and the sampling port is respectively connected to a particle size analyzer and a pH monitor; a discharge port is arranged at the bottom of the reactor.

2. The battery-grade manganese tetraoxide preparation system according to claim 1, characterized in that: The reactor is provided with a stirring structure, which includes multiple layers of stirring paddles, and the diameters of the blades of the multiple layers of stirring paddles decrease from top to bottom.

3. The battery-grade manganese tetraoxide preparation system according to claim 2, characterized in that: The stirring mechanism comprises three layers of stirring paddles, the blades of adjacent stirring paddles are staggered, and the ratio of the blade diameters of the stirring paddles from top to bottom is 2-2.5:1.2-1.8:

1.

4. The battery-grade manganese tetraoxide preparation system according to claim 2, characterized in that: It also includes a controller, and the stirring mechanism, the particle size analyzer, the pH monitor, the first feed pump, the second feed pump, the third feed pump, and the control valve are all electrically connected to the controller.

5. The battery-grade manganese tetraoxide preparation system according to claim 4, characterized in that: It also includes an alarm, which is electrically connected to the controller.

6. The battery-grade manganese tetraoxide preparation system according to claim 4, characterized in that: A temperature sensor is also provided in the reactor, and the temperature sensor is electrically connected to the controller.

7. The battery-grade manganese tetraoxide preparation system according to claim 1, characterized in that: The discharge port of the reactor is connected to a filtering device and a drying device in sequence.

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