Method for synthesizing high-purity manganese acetate
Through the direct reaction of high-purity manganese hydroxide and acetic acid, the problems of high impurities, complex processes and safety hazards in the existing manganese acetate synthesis methods are solved, and the synthesis of high-purity manganese acetate and simplified process flow is realized.
Patent Information
- Application Number
- CN202411652373.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-19
- Publication Date
- 2025-02-25
AI Technical Summary
The existing manganese acetate synthesis methods have problems such as high impurities, complex processes, and safety hazards, which are difficult to meet the requirements of high purity and safety.
High-purity manganese hydroxide is directly reacted with acetic acid, and through a simplified process flow, including the preparation, reaction, solid-liquid separation and crystallization drying of manganese hydroxide slurry suspension, high-purity manganese acetate is obtained.
The synthesis of high-purity manganese acetate has been achieved, the process is simplified, the safety is improved, no new impurity elements are introduced, and the reaction efficiency is improved.
Smart Images
Figure CN119504411A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical synthesis, and more specifically, relates to a method for synthesizing high-purity manganese acetate. Background Art
[0002] Manganese acetate is an organic substance with the chemical formula (CH3COO)2Mn. It is a light red transparent monoclinic crystal that is soluble in water and alcohol. It is mainly used as a catalyst in the production of polyester chips and PTA. It is also used in different reactions, such as the synthesis and polymerization of vinyl esters. In the field of solar energy, manganese acetate is widely used in the preparation of photovoltaic materials. In the field of battery processing, manganese acetate can be used to prepare lithium manganate positive electrode materials or additives with excellent high-temperature performance, thereby improving the battery life and energy density, thereby improving charging efficiency and safety. In the field of new energy, manganese acetate can be used as a bearing lubricant in wind turbines, as a heat transfer medium in geothermal heat pump systems, and as a catalyst in the conversion and utilization of biomass energy.
[0003] The existing methods for synthesizing manganese acetate mainly include the manganese acetate method, manganese carbonate method and pyrolusite method. The manganese acetate method is to synthesize manganese with acetic acid to obtain crude manganese acetate, then add a small amount of activated carbon to remove metal ions such as iron and lead, filter, and evaporate, cool, crystallize and dry the filtrate to obtain the finished product. This method will introduce more impurities and is difficult to remove. At the same time, the amount of distilled water and energy consumption are large, and a large amount of hydrogen will be released during the reaction. The safety level requirements are very high. The manganese carbonate method uses industrial manganese carbonate as raw material and slurries it, adds acetic acid and heats it to above 80°C. reaction, and then the above-mentioned process can be used to obtain the final product; the manganese acetate product obtained by this method has high impurities and cannot meet the battery-grade quality requirements; the pyrolusite method is to use high-grade pyrolusite (Mn02 content greater than 70%) as raw material, and reduce and roast it with anthracite at 850°C to generate Mn0, add it to an acetic acid solution with a concentration of about 15% and heat it to boiling, and then obtain the product after filtration, concentration, crystallization, separation and packaging; however, this synthesis method requires high-grade pyrolusite, and the process is relatively complicated, and toxic and harmful gas H2S must be used, which poses a very large safety hazard.
[0004] Therefore, a method for synthesizing manganese acetate with simple process, clean and safe synthesis process and high purity is needed. Summary of the invention
[0005] The object of the present invention is to provide a method for synthesizing high-purity manganese acetate, which can directly synthesize manganese acetate by using high-purity manganese hydroxide as a raw material and acetic acid, without introducing new impurity elements during the synthesis process, and has a short process and a simple flow, and the obtained high-purity manganese acetate has high purity.
[0006] To achieve the above object, the present invention provides the following technical solutions: A method for synthesizing high-purity manganese acetate of the present invention comprises the following steps: S1. The high-purity manganese hydroxide is prepared into a manganese hydroxide slurry suspension with pure water; S2. The manganese hydroxide slurry suspension and acetic acid are added to the reaction vessel in a ratio of 1:1-5:1 for reaction; S3. After the reaction is completed, the medium in the reaction vessel is separated into solid and liquid, the liquid is a high-purity manganese acetate solution, and the solid is an unreacted manganese hydroxide; S4. Crystallizing and drying the high-purity manganese acetate solution to obtain a high-purity manganese acetate product; The reaction equation of high-purity manganese acetate is: Mn(OH)2+2CH3COOH=Mn(CH3COO)2+2H2O.
[0007] As a further improvement of the present invention, the reaction temperature in the reaction container of step S2 is 25-90°C.
[0008] As a further improvement of the present invention, the reaction time in the reaction container of step S2 is 1-24h.
[0009] As a further improvement of the present invention, the reaction vessel in step S2 includes a reactor, a heating jacket, a stirring device and a filtering device; the reactor includes a reactor body and an end cover, a feeding port is provided on the top of the end cover, and a discharge port is provided at the bottom of the reactor body; the heating jacket is fitted around the outer periphery of the reactor body for heating the inside of the reactor, and the stirring device is detachably mounted on the top of the end cover for stirring the medium inside the reactor; the filtering device is detachably mounted in the area where the discharge port is located, and is used for solid-liquid separation of solid manganese hydroxide and liquid manganese acetate solution in the reactor after the reaction is completed, thereby avoiding the transfer and filtration of the medium inside the reactor and simplifying the processing flow.
[0010] As a further improvement of the present invention, the stirring device includes a stirring motor, a driving shaft and a stirring blade; the output end of the stirring motor is detachably connected to the upper part of the driving shaft, and the stirring blade is detachably installed at the lower part of the driving shaft, and is used to stir the medium inside the reactor to prevent the manganese hydroxide suspension from settling after standing, so that the manganese hydroxide remains in a suspension state, increases the contact area between acetic acid and manganese hydroxide, and improves the reaction efficiency.
[0011] As a further improvement of the present invention, the lower end of the drive shaft extends into the interior of the filter device, and a through hole is opened at the top of the filter device, which is rotatably connected to the outer wall of the drive shaft, so that the drive shaft remains uniform and stable when the stirring blade rotates, avoiding the drive shaft from shifting during rotation and affecting the normal operation of the stirring motor.
[0012] As a further improvement of the present invention, the filtering device includes a filter screen, an upper disk, a lower ring and a backwashing part; the diameter of the upper disk is smaller than the diameter of the lower ring, and the filter screen is arranged between the upper disk and the lower ring in the form of a cone, so that the solid manganese hydroxide falling on the surface of the filter screen falls along the cone to the bottom of the kettle body to avoid blocking subsequent filtration; a through hole is opened at the upper disk, which is rotatably connected to the driving shaft of the stirring device; an installation groove is opened at the bottom of the inner side of the reactor, and the lower ring is embedded and installed in the installation groove; the backwashing part is located inside the filter screen and is detachably connected to the stirring device, and is used to be driven by the stirring device inside the filter device to backwash and impact the precipitation on the surface of the filter screen to avoid the solid manganese hydroxide blocking the filtration of the filter screen.
[0013] As a further improvement of the present invention, the backwash part includes a push plate, a connecting part, a spring and a sliding part; the connecting part is detachably installed at the bottom of the stirring device, the connecting part is provided with a protrusion, which is slidably connected to the inner wall of one end of the sliding part, and the other end of the sliding part is fixedly connected to the push plate; the spring is sleeved on the outer periphery of the protrusion, and the two ends respectively abut the connecting part and the sliding part; a limit block is provided on the top of the push plate, and an elliptical ring platform is provided at the lower part of the upper disk, and the limit block abuts on the inner side of the elliptical ring platform, which is used to make the sliding part slide back and forth along the axial direction where the protrusion is located when the stirring device is stirring, thereby driving the push plate to reciprocate to generate liquid flow to impact the filter mesh surface, thereby ensuring the filtering effect of the filter mesh.
[0014] Compared with the prior art, the invention has the following beneficial effects: a method for synthesizing high-purity manganese acetate of the invention directly synthesizes manganese acetate by using high-purity manganese hydroxide as a raw material and acetic acid, no new impurity elements are introduced in the synthesis process, the process is short, the flow is simple, and the obtained high-purity manganese acetate has high purity; by using a high-purity manganese hydroxide suspension to react with acetic acid, the contact area between manganese hydroxide and acetic acid is increased, and the reaction rate is improved; by arranging a filtering device inside the reaction container, the high-purity manganese acetate solution is discharged from the discharge port, and the process of transferring the material is simplified; by arranging a backwashing part inside the filtering device, the backwashing part is synchronously driven by a stirring device, and a flow medium is released from the inside of the filtering device to the outside of the filtering device to impact the filter screen surface, thereby avoiding the deposition of solid manganese hydroxide on the filter screen surface. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 is a process flow chart of the present invention; Figure 2 It is a schematic diagram of the structure of the reaction container of the present invention; Figure 3 It is a schematic diagram of the cross-sectional structure of the reaction container of the present invention; Figure 4 It is an enlarged schematic diagram of the structure at A of the present invention; Figure 5 It is a schematic diagram of the structure of the filtering device of the present invention.
[0016] Description of the numbers in the figure: 1 reaction kettle, 11 kettle body, 111 discharge port, 12 end cover, 121 feeding port, 2 heating jacket, 3 stirring device, 31 stirring motor, 32 driving shaft, 33 stirring blade, 4 filtering device, 41 filter screen, 42 upper plate, 421 elliptical ring platform, 43 lower ring, 44 backwashing part, 441 push plate, 441 limit block, 442 connecting piece, 443 spring, 444 sliding piece. DETAILED DESCRIPTION
[0017] Specific embodiment 1: Please refer to Figure 1 A method for synthesizing high-purity manganese acetate comprises the following steps: S1. The high-purity manganese hydroxide is prepared into a manganese hydroxide slurry suspension with pure water; S2. The manganese hydroxide slurry suspension and acetic acid are added to the reaction vessel in a ratio of 1:1-5:1 for reaction; S3. After the reaction is completed, the medium in the reaction vessel is separated into solid and liquid, the liquid is a high-purity manganese acetate solution, and the solid is an unreacted manganese hydroxide; S4. Crystallizing and drying the high-purity manganese acetate solution to obtain a high-purity manganese acetate product; The reaction equation of high-purity manganese acetate is: Mn(OH)2+2CH3COOH=Mn(CH3COO)2+2H2O.
[0018] Specifically, the reaction temperature in the reaction container of step S2 is 25-90°C.
[0019] Specifically, the reaction time in the reaction container of step S2 is 1-24h.
[0020] Specifically, the reaction container in step S2 is as follows Figure 2-Figure 3 The reactor 1 includes a reactor body 11 and an end cover 12, wherein a feeding port 121 is provided at the top of the end cover 12 for adding manganese hydroxide suspension and acetic acid into the reactor 1; a discharge port 111 is provided at the bottom of the reactor body 11 for discharging the high-purity manganese acetate solution obtained after the reaction is completed; the heating jacket 2 is fitted on the outer periphery of the reactor body 11 for heating the inside of the reactor 1; the stirring device 3 is detachably mounted on the top of the end cover 12 for stirring the medium inside the reactor 1; the filter device 4 is detachably mounted in the area where the discharge port 111 is located for performing solid-liquid separation on the solid manganese hydroxide and the liquid manganese acetate solution in the reactor 1 after the reaction is completed, thereby avoiding the transfer and filtration of the medium inside the reactor 1 and simplifying the processing flow.
[0021] Specifically, the stirring device 3 includes a stirring motor 31, a driving shaft 32 and a stirring blade 33; the output end of the stirring motor 31 is detachably connected to the upper part of the driving shaft 32, and the stirring blade 33 is detachably installed at the lower part of the driving shaft 32, and is used to stir the medium inside the reactor 1 to prevent the manganese hydroxide suspension from settling after standing, so that the manganese hydroxide remains in a suspension state, increases the contact area between acetic acid and manganese hydroxide, and improves the reaction efficiency.
[0022] Specifically, the lower end of the drive shaft 32 extends into the interior of the filter device 4. A through hole is opened at the top of the filter device 4, which is rotatably connected to the outer wall of the drive shaft 32, so that the drive shaft 32 remains uniform and stable when the stirring blade 33 rotates, avoiding the drive shaft 32 from deviating during rotation and affecting the normal operation of the stirring motor 31.
[0023] Specifically, Figure 4 The filter device 4 shown includes a filter screen 41, an upper disk portion 42, a lower ring portion 43 and a backwash portion 44; the diameter of the upper disk portion 42 is smaller than the diameter of the lower ring portion 43, and the filter screen 41 is arranged between the upper disk portion 42 and the lower ring portion 43 in the form of a cone, so that the solid manganese hydroxide falling on the surface of the filter screen 41 falls along the cone surface to the bottom surface of the kettle body 11, avoiding blocking the subsequent filtration of the filter screen 41; a through hole is opened at the upper disk portion 42, which is rotatably connected to the driving shaft 32 of the stirring device 3; a mounting groove is opened at the bottom of the inner side of the reactor 1, and the lower ring portion 43 is embedded and installed in the mounting groove; the backwash portion 44 is located inside the filter screen 41 and is detachably connected to the driving shaft 32 of the stirring device 3, and is used to be driven by the driving shaft 32 inside the filter device 4 to backwash and impact the precipitation on the surface of the filter screen 41, avoiding the filtration of the filter screen 41 blocked by the solid manganese hydroxide.
[0024] Specifically, Figure 5 The backwashing part 44 shown in the figure includes a push plate 441, a connecting member 442, a spring 443 and a sliding member 444; the connecting member 442 is detachably mounted on the bottom of the driving shaft 32 by means of a shaft key connection, the connecting member 442 is provided with a protrusion, which is slidably connected to the inner wall of one end of the sliding member 444, and the other end of the sliding member 444 is fixedly connected to the push plate 441; the spring 443 is sleeved on the outer periphery of the protrusion, and the two ends respectively contact the connecting member 442 and the sliding member 444; a limit block 4411 is provided on the top of the push plate 441, an elliptical ring platform 421 is provided on the lower part of the upper plate 42, and the limit block 44 11 abuts against the inner side of the elliptical ring stage 421. When the limit block 4411 is close to the short axis of the elliptical ring stage 421, the sliding member 444 slides toward the raised portion of the connecting member 442, compressing the spring 443, and the push plate 441 moves radially toward the inner side of the filter device 4; when the limit block 4411 is close to the long axis of the elliptical ring stage 421, the sliding member 444 slides away from the raised portion of the connecting member 442, the spring 443 elastically expands, and the push plate 441 moves radially toward the outer side of the filter device 4. At this time, a liquid flow is generated to impact the surface of the filter screen 41, thereby ensuring the filtering effect of the filter screen 41.
[0025] During use, high-purity manganese hydroxide and pure water are prepared into a manganese hydroxide suspension, the manganese hydroxide suspension and acetic acid are added into the reactor 1 from the feed port 121, and the inside of the reactor 1 is heated by the heating jacket 2; the stirring motor 31 is turned on to drive the stirring blade 33 to rotate, so as to ensure that the manganese hydroxide suspension remains in a suspended state and increase the contact area between the acetic acid and the manganese hydroxide; the driving shaft 32 is controlled to rotate by the stirring motor 31, thereby driving the connecting piece 442 detachably connected to the driving shaft 32 to rotate accordingly, and the connecting piece 442 is driven during the rotation process. The limit block 4411 at the top of the push plate 441 and the elliptical ring stage 421 at the bottom of the upper disk 42 are guided and restricted, so that the push plate 441 can reciprocate along the axis of the sliding member 443 during the rotation process, thereby generating a liquid flow to impact the surface of the filter screen 41, thereby preventing solid manganese hydroxide from remaining on the surface of the filter screen 41; after the reaction is completed, the solid manganese hydroxide is blocked by the filter screen 41 and remains in the reactor 1, and the filtered liquid manganese acetate solution is discharged from the discharge port 111 and collected, and a high-purity manganese acetate product can be obtained by crystallizing and drying the manganese acetate solution.
[0026] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for synthesizing high-purity manganese acetate, characterized in that: The following steps are involved: S1. The high-purity manganese hydroxide is prepared into a manganese hydroxide slurry suspension with pure water; S2. The manganese hydroxide slurry suspension and acetic acid are added to the reaction vessel in a ratio of 1:1-5:1 for reaction; S3. After the reaction is completed, the medium in the reaction vessel is separated into solid and liquid, the liquid is a high-purity manganese acetate solution, and the solid is an unreacted manganese hydroxide; S4. Crystallize and dry the high-purity manganese acetate solution to obtain a high-purity manganese acetate product.
2. A method for synthesizing high-purity manganese acetate according to claim 1, characterized in that: The reaction temperature in the reaction vessel of step S2 is 25-90°C.
3. A method for synthesizing high-purity manganese acetate according to claim 1, characterized in that: The reaction time of step S2 is 1-24h.
4. A method for synthesizing high-purity manganese acetate according to claim 1, characterized in that: The reaction vessel in step S2 comprises a reactor (1), a heating jacket (2), a stirring device (3) and a filtering device (4); the reactor (1) comprises a reactor body (11) and an end cover (12); a feeding port (121) is provided at the top of the end cover (12), and a discharge port (111) is provided at the bottom of the reactor body (11); the heating jacket (2) is sleeved on the outer periphery of the reactor body (11) and is used to heat the inside of the reactor (1); the stirring device (3) is detachably mounted on the top of the end cover (12) and is used to stir the medium inside the reactor (1); the filtering device (4) is detachably mounted in the area where the discharge port (111) is located and is used to perform solid-liquid separation on the medium inside the reactor (1) after the reaction is completed.
5. A method for synthesizing high-purity manganese acetate according to claim 4, characterized in that: The stirring device (3) comprises a stirring motor (31), a driving shaft (32) and a stirring blade (33); the output end of the stirring motor (31) is detachably connected to the upper part of the driving shaft (32), and the stirring blade (33) is detachably mounted on the lower part of the driving shaft (32) and is used to stir the medium inside the reaction kettle (1); the lower end of the driving shaft (32) extends into the interior of the filtering device (4), and a through hole is formed on the top of the filtering device (4) and is rotatably connected to the outer wall of the driving shaft (32) to ensure uniform rotation of the stirring device (3).
6. A method for synthesizing high-purity manganese acetate according to claim 4, characterized in that: The filter device (4) comprises a filter screen (41), an upper disk (42), a lower ring (43) and a backwashing portion (44); the diameter of the upper disk (42) is smaller than the diameter of the lower ring (43); the filter screen (41) is arranged between the upper disk (42) and the lower ring (43) in the form of a cone; a through hole is provided at the upper disk (42) and is rotatably connected to the stirring device (3); a mounting groove is provided at the bottom of the inner side of the reaction kettle (1); the lower ring (43) is embedded and installed in the mounting groove; the backwashing portion (44) is located inside the filter screen (41) and is detachably connected to the stirring device (3) and is used for backwashing the sediment on the surface of the impact filter screen (41) inside the filter device (4).
7. A method for synthesizing high-purity manganese acetate according to claim 6, characterized in that: The backwashing part (44) comprises a push plate (441), a connecting member (442), a spring (443) and a sliding member (444); the connecting member (442) is detachably mounted on the bottom of the stirring device (3); the connecting member (442) is provided with a protrusion, which is slidably connected to the inner wall of one end of the sliding member (444); the other end of the sliding member (444) is fixedly connected to the push plate (441); the spring (443) is sleeved on the outer periphery of the protrusion, and its two ends respectively abut against the connecting member (442) and the sliding member (444); a limit block (4411) is provided on the top of the push plate (441), and an elliptical ring platform (421) is provided on the lower part of the upper plate (42); the limit block (4411) abuts against the inner side of the elliptical ring platform (421), and is used for causing the sliding member (444) to drive the push plate (441) to slide back and forth along the axial direction of the protrusion when the stirring device (3) is stirring, so as to generate a liquid flow to impact the surface of the filter screen (41).