A high-purity manganese sulfate purification device

Abstract

The utility model relates to the technical field of manganese sulfate production, especially a high -purity manganese sulfate purification device for making manganese sulfate solution carry out chemical precipitation purification, connecting with filter press module and extraction module in proper order, and including: the jar body has the working cavity in the inside, the top of jar body is equipped with the liquid inlet pipe, and the liquid inlet pipe communicates with solution pipe and reagent pipe, the mixing mechanism includes spiral mixing spare, ultrasonic oscillation subassembly and mixing wall, spiral mixing spare sets up at the top of working cavity and communicates with liquid inlet pipe, and mixing wall surrounds spiral mixing spare and sets up and combines and encloses and forms the cladding cavity, and mixing wall top interval is equipped with mixed liquor export, ultrasonic oscillation subassembly sets up in the cladding cavity, and the liquid in liquid inlet pipe flows through spiral mixing spare and then enters the cladding cavity, and after the oscillation of ultrasonic oscillation group, the mixed liquor export flows out, the stirring mechanism sets up at the bottom of working cavity, and the solution of mixing mechanism is stirred. The utility model can make the solution mix fully, improve the purification effect and efficiency.

Description

Technical Field

[0001] This utility model relates to the field of manganese sulfate production technology, and in particular to a high-purity manganese sulfate purification device. Background Technology

[0002] Manganese sulfate is classified into high-purity manganese sulfate and standard manganese sulfate according to purity, namely battery grade and feed grade. Battery-grade manganese sulfate is mainly used to manufacture high-purity electrolytic manganese dioxide, manganese tetroxide, ternary precursors and other battery materials. The production routes of high-purity manganese sulfate mainly include acid leaching method and two-ore one-step method. In both of the mainstream production routes, the products in the process need to be purified to remove impurities.

[0003] The main methods for removing impurities and purifying manganese sulfate in the market are recrystallization and chemical precipitation. Recrystallization involves repeatedly crystallizing to gradually separate impurity ions from the manganese sulfate solution, thereby obtaining high-purity manganese sulfate. Chemical precipitation, on the other hand, involves adding various reagents such as fluorides to precipitate impurities, followed by extraction and defluorination to obtain high-purity manganese sulfate.

[0004] Due to cost considerations, chemical precipitation is the primary purification method used in the production of high-purity manganese sulfate. However, the final residue requirements for high-purity manganese sulfate are high. Conventional reaction equipment only uses a stirring paddle to mix the solution, and the time required to achieve uniform mixing is long, resulting in low overall purification efficiency. Furthermore, the stirring method causes the liquid within the reaction equipment to rotate synchronously under centrifugal force. This centrifugal force varies with the distance from the stirring paddle, leading to lower force at the edges and uneven mixing distribution. Consequently, some solutions may not be fully mixed, resulting in insufficient final purification. Utility Model Content

[0005] The technical problem to be solved by this utility model is to provide a high-purity manganese sulfate purification device, which solves the problem that the existing purification equipment has a simple mixing method, resulting in insufficient purification effect and low purification efficiency.

[0006] To solve the above-mentioned technical problems, the technical solution adopted by this utility model is as follows: a high-purity manganese sulfate purification device, used for chemical precipitation purification of manganese sulfate solution, connected sequentially to a pressure filtration module and an extraction module, comprising:

[0007] The tank has an internal working chamber, and the top of the tank is equipped with a liquid inlet pipe, which is connected to the solution pipe and the reagent pipe.

[0008] The mixing mechanism includes a spiral mixer, an ultrasonic oscillation assembly, and a mixing wall. The spiral mixer is located at the top of the working chamber and communicates with the inlet pipe. The spiral mixer is used to initially mix the liquid coming from the inlet pipe. The mixing wall surrounds the spiral mixer and encloses it to form a covered cavity. The top of the mixing wall is provided with a mixed liquid outlet at intervals. The ultrasonic oscillation assembly is located in the covered cavity. The liquid in the inlet pipe flows through the spiral mixer and enters the covered cavity. After being oscillated by the ultrasonic oscillation assembly, it flows out from the mixed liquid outlet.

[0009] The stirring mechanism is located at the bottom of the working chamber and stirs the solution flowing out of the mixing mechanism.

[0010] In one embodiment, the ultrasonic oscillation assembly includes an ultrasonic generating module, an oscillation plate, and an extended ring wall. The ultrasonic generating module is disposed on the mixing wall directly below the helical mixing component, the oscillation plate is disposed on the ultrasonic generating module, and the extended ring wall surrounds the helical mixing component and extends vertically upward from the oscillation plate.

[0011] In one embodiment, the oscillating plate is provided with multiple levels of extended annular walls from the center outward, and multiple levels of spacer annular walls are provided between the multiple levels of extended annular walls.

[0012] In one embodiment, a spacer ring wall is provided between the extended ring wall and the mixing wall in the enclosed cavity. The spacer ring wall extends downward from the top of the working cavity and is spaced apart from the oscillating plate. The top of the extended ring wall is spaced apart from the top of the tank and forms a corresponding S-shaped circulation channel with the mixing wall and the spacer ring wall.

[0013] In one embodiment, a sealing ring is fitted onto the oscillating plate, and the sealing ring is sealed to the mixing wall.

[0014] In one embodiment, the mixing wall and the extension ring wall are provided with waste liquid outlets, and the height of the waste liquid outlets is higher than the height of the sealing ring.

[0015] In one embodiment, the spiral mixing component includes a mixing tube and a spiral guide plate, the spiral guide plate being disposed inside the mixing tube.

[0016] In one embodiment, the spiral guide plate includes a first spiral element and a second spiral element, the spiral directions of the first spiral element and the second spiral element being opposite, and the first spiral element and the second spiral element being alternately arranged.

[0017] In one embodiment, the stirring mechanism includes at least two stages of blades with different deflection directions.

[0018] The beneficial effects of this invention are as follows: Traditional reaction vessels mainly use stirring devices to mix the liquid inside the vessel. However, during the stirring process, uneven distribution of reagents may result in high-fluoride and low-fluoride zones. In high-fluoride zones, excess fluoride ions may form colloidal manganese fluoride precipitates, which encapsulate unreacted calcium and magnesium ions, reducing the efficiency of impurity removal. In low-fluoride zones, the fluoride ion concentration is insufficient, and calcium and magnesium ions cannot be completely precipitated as CaF2 and MgF2, leading to residual impurities entering subsequent processes and affecting the purification effect. At the same time, fluoride precipitate agglomerates are easily formed in the dead stirring areas, encapsulating manganese sulfate or unreacted calcium and magnesium ions, making it difficult to remove impurities during washing. Furthermore, the precipitate particles generated by uneven stirring are of mixed coarse and fine sizes, which can easily cause filter cake caking in the subsequent filter press module, clogging the filter channels, prolonging the solid-liquid separation time, and ultimately affecting the purification effect and efficiency.

[0019] This invention features a mixing mechanism at the top of the working chamber. A spiral mixer initially mixes the liquid from the inlet pipe. Through its internal mechanical structure, the spiral mixer causes the liquid to circulate and be divided multiple times along its internal channels, achieving a guiding effect that eliminates the need for external power, thus reducing operating costs while ensuring effective initial mixing. The mixed solution then enters a cavity enclosed by the mixing wall. An ultrasonic oscillation component within this cavity further mixes the initially mixed solution. The liquid in the cavity is continuously subjected to ultrasonic oscillation during its ascent, eliminating mechanical dead zones and ensuring thorough mixing of the manganese sulfate solution and fluoride reagent. Simultaneously, the resulting precipitate does not agglomerate under ultrasonic oscillation, effectively preventing the formation of fluoride precipitate agglomerates, reducing the pressure on subsequent filtration and separation, and ultimately improving purification efficiency.

[0020] Although the mixing mechanism can thoroughly mix the manganese sulfate solution with the fluoride reagent, in mass production, the time for the solution to flow through the spiral mixer and ultrasonic oscillation assembly is relatively short, and the process of complete precipitation and stabilization requires a considerable amount of time. To ensure sufficient overall reaction time, complete removal of impurities, and without affecting the mixing efficiency of the mixing mechanism, this invention allows the homogeneous solution after ultrasonic oscillation to flow into the working chamber through the mixed liquid outlet at the top of the mixing wall, where it undergoes a thorough reaction. Simultaneously, as precipitation gradually increases during the reaction, to prevent precipitate aggregation and caking, this invention incorporates a stirring mechanism at the bottom of the working chamber. This ensures the solution within the working chamber remains in a flowing state, allowing the generated precipitate to flow with the solution into the subsequent pressure filtration module for recovery. This reduces the frequency of cleaning the bottom precipitate, prevents corrosion of the high-purity manganese sulfate purification device by water during cleaning, thereby extending the overall service life of this invention and reducing maintenance costs. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a schematic diagram of the structure of an embodiment of the present utility model;

[0023] Figure 2 This is a schematic diagram of the mixing mechanism in one embodiment of the present invention;

[0024] Figure 3 This is a schematic diagram of the overall process of an embodiment of the present utility model.

[0025] Label Explanation:

[0026] 1. Tank body; 11. Working chamber; 12. Inlet pipe; 13. Solution pipe; 14. Reagent pipe; 2. Mixing mechanism; 21. Spiral mixing component; 211. Mixing pipe; 212. Spiral guide plate; 2121. First spiral element; 2122. Second spiral element; 22. Ultrasonic oscillation assembly; 221. Ultrasonic generating module; 222. Oscillating plate; 223. Extending ring wall; 224. Sealing ring; 23. Mixing wall; 231. Mixed liquid outlet; 24. Encapsulated cavity; 25. Spacer ring wall; 26. Flow gap; 27. Waste liquid outlet; 3. Stirring mechanism; 4. Filtration module; 5. Extraction module. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0028] In the description of this utility model, it should be noted that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings and are only for the convenience of describing this utility model and simplifying the description. They 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, and therefore should not be construed as a limitation on this utility model. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0029] Please refer to Figures 1 to 3 A high-purity manganese sulfate purification device, used for chemical precipitation purification of manganese sulfate solution, is sequentially connected to a pressure filtration module 4 and an extraction module 5, comprising:

[0030] The tank body 1 has a working chamber 11 inside. An inlet pipe 12 is located at the top of the tank body 1, and the inlet pipe 12 is connected to a solution pipe 13 and a reagent pipe 14. Specifically, the solution pipe 13 is used to deliver manganese sulfate solution, and the reagent pipe 14 is used to deliver fluoride reagent. Those skilled in the art can adjust the flow rate ratio of the solution pipe 13 and the reagent pipe 14 as needed to control the fluoride concentration; no specific limitations are made.

[0031] The mixing mechanism 2 includes a spiral mixer 21, an ultrasonic oscillation assembly 22, and a mixing wall 23. The spiral mixer 21 is located at the top of the working chamber 11 and communicates with the inlet pipe 12. The spiral mixer 21 is used to initially mix the liquid coming from the inlet pipe 12. The mixing wall 23 surrounds the spiral mixer 21 and forms a covered cavity 24. The top of the mixing wall 23 is provided with a mixed liquid outlet 231 at intervals. The ultrasonic oscillation assembly 22 is located inside the covered cavity 24. The liquid in the inlet pipe 12 flows through the spiral mixer 21 and enters the covered cavity 24. After being oscillated by the ultrasonic oscillation assembly 22, it flows out from the mixed liquid outlet 231. The stirring mechanism 3 is located at the bottom of the working chamber 11 and stirs the solution flowing out of the mixing mechanism 2.

[0032] After setting up the ultrasonic module, if oscillation is only performed at the bottom of the encapsulated cavity 24, although the solution can be mixed evenly, the precipitate gradually formed during the solution's ascent receives less ultrasonic stimulation, potentially leading to aggregates. Furthermore, in large-scale production processes, the solution flow rate is high, and the liquid level rises rapidly within the encapsulated cavity 24, resulting in a shorter duration of ultrasonic oscillation per unit volume of liquid. Therefore, the ultrasonic oscillation assembly 22 of this invention includes an ultrasonic generating module 221, an oscillating plate 222, and an extending annular wall 223. The ultrasonic generating module 221 is positioned on the mixing wall 23 directly below the spiral mixer 21, the oscillating plate 222 is positioned on the ultrasonic generating module 221, and the extending annular wall 223 surrounds the spiral mixer 21 and extends vertically upwards from the oscillating plate 222. This extends the annular wall 223, dividing the encapsulated cavity 24 and lengthening the solution's path within it. This ensures that the solution maintains close contact with the ultrasonic module during flow, preventing attenuation of ultrasonic oscillation and guaranteeing uniform mixing and separation of precipitates. Specifically, the ultrasonic generating module 221 includes structures such as an ultrasonic generator and a transducer. Those skilled in the art can select a suitable ultrasonic generating module 221 as needed to make the oscillating plate 222 vibrate, without making specific limitations.

[0033] After the extended annular wall 223 is set, the liquid flowing through the spiral mixer 21 enters the area formed by the extended annular wall 223 and rises. After falling from the top of the extended annular wall 223, it continues to rise and flows out from the mixed liquid outlet 231. However, when the solution between the extended annular wall 223 and the mixing wall 23 is full, the subsequent solution will flow directly from the top of the extended annular wall 223 to the mixed liquid outlet 231, preventing the solution between the extended annular wall 223 and the mixing wall 23 from entering the subsequent process. Therefore, in this embodiment, a spacer annular wall 25 is also provided in the enclosing cavity 24 between the extended annular wall 223 and the mixing wall 23. The spacer annular wall 25 extends downward from the top of the working cavity 11 and is spaced apart from the oscillating plate 222. The top of the extended annular wall 223 is spaced apart from the top of the tank 1, and forms a corresponding S-shaped circulation channel with the mixing wall 23 and the spacer annular wall 25. The spacer annular wall 25 blocks the direct flow path of the extended annular wall 223 to the mixed liquid outlet 231, ensuring that the flow of the solution within the enclosed cavity 24 meets the requirements. Specifically, in the vertical direction, the projection area of ​​the spacer annular wall 25 is within the projection area of ​​the oscillating plate 222. This arrangement allows the solution between the spacer annular wall 25 and the mixing wall 23 to be subjected to ultrasonic action, enabling continuous oscillation during flow and ensuring a good dispersion and mixing effect. Specifically, there is a flow gap 26 between the spacer annular wall 25 and the oscillating plate 222, and between the extended annular wall 223 and the top of the working cavity 11. The spacer annular wall 25, the extended annular wall 223, and the mixing wall 23 together form a circulating flow channel. Specifically, the size of the flow gap 26 can be adjusted by those skilled in the art as needed and is not specifically limited.

[0034] Preferably, the oscillating plate 222 is provided with multi-level extended annular walls 223 from the center outward, and multi-level spaced annular walls 25 are provided between the multi-level extended annular walls 223, thereby increasing the number of cycles in the circulating channel and further enhancing the mixing effect. Those skilled in the art can adjust it as needed, without making specific limitations.

[0035] The ultrasonic generating module 221 of the ultrasonic oscillation assembly 22 is disposed between the oscillation plate 222 and the mixing wall 23. To prevent solution or precipitate from entering the ultrasonic generating module 221 and causing damage, in this embodiment, a sealing ring 224 is fitted on the oscillation plate 222, and the sealing ring 224 is sealed to the mixing wall 23. The sealing ring 224 seals the area below the oscillation plate 222, forming an installation area. The ultrasonic generating module 221 or other components requiring protection can be centrally located in the installation area. This not only prevents damage to the ultrasonic generating module 221, but also prevents rigid contact between the oscillation plate 222 and the mixing wall 23, thus avoiding damage to the oscillation plate 222 or the mixing wall 23 during long-term use. During maintenance, only the sealing ring 224 needs to be replaced, thereby improving the overall service life and reducing maintenance costs.

[0036] In this embodiment, the mixing wall 23 and the extending ring wall 223 are provided with waste liquid outlets 27, and the height of the waste liquid outlets 27 is higher than the height of the sealing ring 224. The waste liquid outlets 27 are provided so that the solution inside the enclosing cavity 24 can flow out when the machine is stopped, thus preventing the solution from corroding the mixing mechanism 2.

[0037] Preferably, a solenoid valve is provided on the waste liquid outlet 27. Those skilled in the art can open or close the solenoid valve at different positions as needed, thereby changing the flow path of the solution in the enclosed cavity 24 and adjusting the time when the solution is subjected to ultrasound.

[0038] In this embodiment, the spiral mixing component 21 includes a mixing tube 211 and a spiral guide plate 212, with the spiral guide plate 212 disposed inside the mixing tube 211. Those skilled in the art can select a suitable spiral guide plate 212 as needed.

[0039] In this embodiment, the spiral guide plate 212 includes a first spiral element 2121 and a second spiral element 2122. The spiral directions of the first spiral element 2121 and the second spiral element 2122 are opposite, and the first spiral element 2121 and the second spiral element 2122 are alternately arranged. Specifically, the torsion angle of the first spiral element 2121 and the second spiral element 2122 is 180° or 270°.

[0040] A single-layer stirring impeller creates laminar flow in the edge region of the solution within the working chamber 11. As precipitate gradually forms in the solution, the laminar flow prevents the precipitate from rising within the solution. Therefore, the stirring mechanism 3 includes at least two stages of impellers with different deflection directions. Turbulence is created by the impellers at different angles, preventing the precipitate from settling.

[0041] Preferably, the stirring mechanism 3 includes horizontal blades and vertical blades, which form turbulence and disturbance through blades in different directions to avoid sedimentation, settling and caking.

[0042] Although this document uses terms such as tank body and working cavity frequently, the possibility of using other terms is not excluded. These terms are used merely for the convenience of describing and explaining the essence of this invention; interpreting them as any additional limitation would contradict the spirit of this invention.

[0043] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model.

Claims

1. A high-purity manganese sulfate purification device, used for chemical precipitation purification of manganese sulfate solution, connected sequentially to a pressure filtration module (4) and an extraction module (5), characterized in that, include: The tank (1) has a working chamber (11) inside. The top of the tank (1) is provided with a liquid inlet pipe (12), which is connected to the solution pipe (13) and the reagent pipe (14). The mixing mechanism (2) includes a spiral mixing component (21), an ultrasonic oscillation assembly (22), and a mixing wall (23). The spiral mixing component (21) is disposed at the top of the working chamber (11) and communicates with the inlet pipe (12). The spiral mixing component (21) is used to perform preliminary mixing of the liquid coming from the inlet pipe (12). The mixing wall (23) is disposed around the spiral mixing component (21) and encloses a cavity (24). The top of the mixing wall (23) is provided with a mixed liquid outlet (231) at intervals. The ultrasonic oscillation assembly (22) is disposed in the cavity (24). The liquid in the inlet pipe (12) flows through the spiral mixing component (21) and enters the cavity (24). After being oscillated by the ultrasonic oscillation assembly (22), it flows out from the mixed liquid outlet (231). A stirring mechanism (3) is located at the bottom of the working chamber (11) to stir the solution flowing out of the mixing mechanism (2).

2. The high-purity manganese sulfate purification apparatus according to claim 1, characterized in that: The ultrasonic oscillation assembly (22) includes an ultrasonic generating module (221), an oscillating plate (222), and an extending annular wall (223). The ultrasonic generating module (221) is disposed on the mixing wall (23) directly below the spiral mixing component (21). The oscillating plate (222) is disposed on the ultrasonic generating module (221). The extending annular wall (223) surrounds the spiral mixing component (21) and extends vertically upward from the oscillating plate (222).

3. The high-purity manganese sulfate purification apparatus according to claim 2, characterized in that: The enclosed cavity (24) is provided with a spacer ring wall (25) between the extended ring wall (223) and the mixing wall (23). The spacer ring wall (25) extends downward from the top of the working cavity (11) and is spaced apart from the oscillating plate (222). The top of the extended ring wall (223) is spaced apart from the top of the tank (1) and forms a corresponding S-shaped circulation channel with the mixing wall (23) and the spacer ring wall (25).

4. The high-purity manganese sulfate purification apparatus according to claim 3, characterized in that: The oscillating plate (222) has multiple levels of extended annular walls (223) arranged from the center outward, and multiple levels of spacer annular walls (25) are arranged between the multiple levels of extended annular walls (223).

5. The high-purity manganese sulfate purification apparatus according to claim 2, characterized in that: A sealing ring (224) is fitted on the oscillating plate (222), and the sealing ring (224) is sealed to the mixing wall (23).

6. The high-purity manganese sulfate purification apparatus according to claim 5, characterized in that: Waste liquid outlet (27) is provided on the mixing wall (23) and the extension ring wall (223), and the height of the waste liquid outlet (27) is higher than the height of the sealing ring (224).

7. The high-purity manganese sulfate purification apparatus according to claim 1, characterized in that: The spiral mixing component (21) includes a mixing tube (211) and a spiral guide plate (212), the spiral guide plate (212) being disposed inside the mixing tube (211).

8. The high-purity manganese sulfate purification apparatus according to claim 7, characterized in that: The spiral guide plate (212) includes a first spiral element (2121) and a second spiral element (2122). The spiral directions of the first spiral element (2121) and the second spiral element (2122) are opposite, and the first spiral element (2121) and the second spiral element (2122) are alternately arranged.

9. The high-purity manganese sulfate purification apparatus according to claim 1, characterized in that: The stirring mechanism (3) includes at least two stages of blades with different deflection directions.

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