Preparation method of high-purity manganese oxalate
By controlling the reaction conditions and steps in the preparation of manganese oxalate, the problems of low purity, high cost and environmental pollution in traditional methods are solved, and the low cost preparation and environmentally friendly production of high-purity manganese oxalate are achieved.
Patent Information
- Application Number
- CN202411316460.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-20
- Publication Date
- 2024-12-27
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The traditional preparation method of manganese oxalate has problems such as low product purity, high cost and serious environmental pollution.
Manganese salt and oxalic acid solution are prepared, the reaction temperature and pH value are controlled, and manganese oxalate precipitation is formed by slow dropping addition and stirring, and then filtered, washed and dried, and finally crushed and sieved to obtain high-purity manganese oxalate.
The preparation of high-purity manganese oxalate is achieved, which reduces production costs and reduces environmental pollution, and ensures the stability of product quality through precise control of reaction conditions.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field related to chemical material preparation, and specifically relates to a method for preparing high-purity manganese oxalate. Background Art
[0002] Manganese oxalate is an important inorganic compound, which is widely used in batteries, catalysts, pigments and other fields. Traditional methods for preparing manganese oxalate mainly include precipitation method, electrolysis method and thermal decomposition method. However, these methods usually have problems such as low product purity, high cost and serious environmental pollution. Therefore, it is of great practical significance to develop an efficient, environmentally friendly and low-cost method for preparing high-purity manganese oxalate. Summary of the invention
[0003] The object of the present invention is to provide a method for preparing high-purity manganese oxalate to solve the problems of low product purity, high cost and serious environmental pollution proposed in the above background technology.
[0004] To achieve the above object, the present invention provides the following technical solutions:
[0005] A method for preparing high-purity manganese oxalate, the preparation method is as follows:
[0006] Prepare a manganese salt solution: weigh 1-5 parts of manganese salt and dissolve it in deionized water to prepare a manganese salt solution of a certain concentration;
[0007] Prepare oxalic acid solution: weigh 2-10 parts of oxalic acid and dissolve them in deionized water to prepare an oxalic acid solution of a certain concentration;
[0008] Mixing reaction: slowly drop the oxalic acid solution into the manganese salt solution while stirring, control the reaction temperature between 20-60°C, and keep the pH value within the range of 3-7, so that the oxalic acid reacts with the manganese salt to generate manganese oxalate precipitate;
[0009] Separation of precipitate: When the reaction is complete, let the mixture stand for a while, then separate the manganese oxalate precipitate from the solution by filtration or centrifugation;
[0010] Washing the precipitate: Wash the separated manganese oxalate precipitate with deionized water several times to remove residual ions and impurities;
[0011] Drying the precipitate: drying the washed manganese oxalate precipitate in an oven, or drying it naturally at room temperature until dry manganese oxalate powder is obtained;
[0012] Post-processing: As needed, the dried manganese oxalate is crushed and sieved to obtain a product of the desired particle size.
[0013] Preferably, the specific steps of preparing the manganese salt solution are as follows:
[0014] Select appropriate manganese salt: According to the requirements of the target product, select appropriate manganese salt, including manganese sulfate and manganese chloride, pre-treat the manganese salt, and remove impurities by heating or filtering to improve the reaction efficiency and the purity of the final product;
[0015] Concentration of solution: According to actual needs, accurately calculate the concentration of manganese salt solution, usually expressed as molar concentration;
[0016] pH value of the solution: Use a buffer solution to control the pH value of the reaction system, so that the required pH environment can be maintained more accurately to facilitate the dissolution of the manganese salt and subsequent reactions;
[0017] Temperature control: Control the temperature of the solution to avoid premature precipitation or decomposition of manganese salts;
[0018] Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration;
[0019] Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
[0020] Preferably, the specific steps of preparing the oxalic acid solution are as follows:
[0021] Select appropriate oxalic acid: According to actual needs, select appropriate oxalic acid, including oxalic acid dihydrate or anhydrous oxalic acid, pre-treat the oxalic acid, and remove impurities by heating or filtering to improve the reaction efficiency and the purity of the final product;
[0022] Solution concentration: Accurately calculate the concentration of oxalic acid solution according to actual needs, usually expressed in molar concentration;
[0023] pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of oxalic acid and subsequent reactions;
[0024] Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of oxalic acid;
[0025] Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration;
[0026] Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
[0027] Preferably, the specific steps of the mixing reaction are as follows:
[0028] Choose the right reactants: Choose the right reactants based on the needs of the target product;
[0029] Solution concentration: Accurately calculate the concentration of reactants according to actual needs;
[0030] pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of the reactants and subsequent reactions;
[0031] Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of the reactants;
[0032] Impurity removal: Remove impurities from the solution by appropriate methods such as centrifugation and filtration;
[0033] Precipitation process: The precipitation process is carried out at a lower temperature, which can promote the formation of larger crystals and reduce the inclusion of impurities, thereby improving the purity of manganese oxalate. The introduction of ultrasonic treatment during the precipitation process can accelerate the precipitation rate, improve the morphology of the crystals, and may increase the purity of the product;
[0034] Reaction stability: Ensure the stability of the reaction during storage and use to avoid changes in properties caused by long-term storage.
[0035] Preferably, the specific steps of washing the precipitate are as follows:
[0036] Select appropriate washing solution: Select appropriate washing solution according to the properties of manganese oxalate precipitate to reduce the dissolution loss of manganese oxalate precipitate and avoid the formation of colloid;
[0037] Optimize the number of washing times: Determine the best number of washing times based on the properties of the manganese oxalate precipitate and the required purity. Excessive washing may result in loss of the manganese oxalate precipitate, while too few washing times may not achieve the required purity standard.
[0038] Control the amount of detergent: Adding an appropriate amount of detergent can ensure the washing effect and avoid the loss caused by excessive washing;
[0039] Use appropriate equipment: Use appropriate equipment and tools, including funnels and glass rods, to ensure accuracy and safety of the washing process;
[0040] Vacuum filtration: Use vacuum filtration equipment to separate the precipitate and mother liquor, which can more effectively remove solvents and impurities;
[0041] Repeat washing: After the first washing, it is necessary to repeat the washing several times to ensure that the impurities on the surface of the manganese oxalate precipitate are thoroughly washed away;
[0042] Drying the manganese oxalate precipitate: After washing, drying the manganese oxalate under vacuum conditions can reduce the drying temperature and prevent thermal decomposition, thereby maintaining the stability and purity of the product for subsequent processing and analysis.
[0043] Preferably, the drying and precipitation step is suggested as follows:
[0044] Select appropriate drying equipment: According to the properties of manganese oxalate precipitate and experimental requirements, select appropriate drying equipment, including oven and dryer;
[0045] Control drying temperature and time: According to the properties of manganese oxalate precipitate, reasonably set the drying temperature and time to avoid overheating that may cause decomposition or deformation of manganese oxalate precipitate;
[0046] Evenly distribute the manganese oxalate precipitate: Before drying, ensure that the manganese oxalate precipitate is evenly distributed in the container to improve drying efficiency;
[0047] Monitor the drying process: During the drying process, the state of the manganese oxalate precipitate should be checked regularly and the drying parameters should be adjusted in time to ensure the drying effect;
[0048] Preferably, the specific steps of the post-processing are as follows:
[0049] Choose the right crushing equipment: According to the physical properties of manganese oxalate and the required particle size, choose the most suitable crushing equipment, including hammer crusher, ball mill, and control the particle size and surface modification of the dried manganese oxalate through mechanical grinding, ball milling or other crushing techniques;
[0050] Control the pulverization time: Properly control the pulverization time to avoid the loss of manganese oxalate caused by excessive pulverization, while ensuring that the required particle size can be achieved;
[0051] Screening treatment: Use sieves with different apertures for graded screening to separate manganese oxalate powder that meets specific particle size requirements;
[0052] Optimize the process: Integrate the drying, crushing and screening steps into one continuous process to improve efficiency and reduce costs by reducing manual operations.
[0053] Compared with the prior art, the present invention provides a method for preparing high-purity manganese oxalate, which has the following characteristics:
[0054] Beneficial effects:
[0055] By optimizing the raw material ratio and reaction conditions, high-purity manganese oxalate can be obtained to meet the requirements of specific applications;
[0056] During the entire preparation process, key parameters such as reaction temperature, pH value, concentration, etc. can be precisely controlled to ensure the stability of product quality;
[0057] Use vacuum filtration equipment to separate the precipitate and the mother liquor, which can more effectively remove the solvent and impurities;
[0058] The pH value of the reaction system is controlled by using a buffer solution instead of directly adjusting the acidity, so as to facilitate the dissolution of oxalic acid and subsequent reactions, thereby improving the purity and efficiency of the preparation;
[0059] The preparation method is applicable to different types of manganese salts and oxalic acid and has good versatility and flexibility. DETAILED DESCRIPTION
[0060] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0061] The present invention provides a technical solution:
[0062] Embodiment 1
[0063] A method for preparing high-purity manganese oxalate, the preparation method is as follows:
[0064] Prepare manganese salt solution: weigh 1 part of manganese salt (such as manganese sulfate MnSO 4 ·H 2 O), dissolved in deionized water to prepare a manganese salt solution of a certain concentration;
[0065] Prepare oxalic acid solution: weigh 2 parts oxalic acid (e.g. oxalic acid dihydrate C 2 H 2 O 4 ·2H 2 O), dissolved in deionized water to prepare an oxalic acid solution of a certain concentration;
[0066] Mixing reaction: slowly add the oxalic acid solution to the manganese salt solution while stirring, control the reaction temperature at 20°C, maintain the pH value at 3, and the oxalic acid reacts with the manganese salt to form manganese oxalate precipitate;
[0067] Separation of precipitate: When the reaction is complete, let the mixture stand for a while, then separate the manganese oxalate precipitate from the solution by filtration or centrifugation;
[0068] Washing the precipitate: Wash the separated manganese oxalate precipitate with deionized water three times to remove residual ions and impurities;
[0069] Drying the precipitate: drying the washed manganese oxalate precipitate in an oven, or drying it naturally at room temperature until dry manganese oxalate powder is obtained;
[0070] Post-processing: As needed, the dried manganese oxalate is crushed and sieved to obtain a product of the desired particle size.
[0071] The specific steps of preparing the manganese salt solution are as follows:
[0072] Select appropriate manganese salt: According to the requirements of the target product, select appropriate manganese salt, including manganese sulfate and manganese chloride, pre-treat the manganese salt, and remove impurities by heating or filtering to improve the reaction efficiency and the purity of the final product;
[0073] Concentration of solution: According to actual needs, accurately calculate the concentration of manganese salt solution, usually expressed as molar concentration;
[0074] pH value of the solution: Use a buffer solution to control the pH value of the reaction system, so that the required pH environment can be maintained more accurately to facilitate the dissolution of the manganese salt and subsequent reactions;
[0075] Temperature control: Control the temperature of the solution to avoid premature precipitation or decomposition of manganese salts;
[0076] Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration;
[0077] Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
[0078] The specific steps of preparing the oxalic acid solution are as follows:
[0079] Select appropriate oxalic acid: According to actual needs, select appropriate oxalic acid, including oxalic acid dihydrate or anhydrous oxalic acid, pre-treat the oxalic acid, and remove impurities by heating or filtering to improve the reaction efficiency and the purity of the final product;
[0080] Solution concentration: Accurately calculate the concentration of oxalic acid solution according to actual needs, usually expressed in molar concentration;
[0081] pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of oxalic acid and subsequent reactions;
[0082] Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of oxalic acid;
[0083] Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration;
[0084] Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
[0085] The specific steps of the mixed reaction are as follows:
[0086] Choose the right reactants: Choose the right reactants based on the needs of the target product;
[0087] Solution concentration: Accurately calculate the concentration of reactants according to actual needs;
[0088] pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of the reactants and subsequent reactions;
[0089] Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of the reactants;
[0090] Impurity removal: Remove impurities from the solution by appropriate methods such as centrifugation and filtration;
[0091] Precipitation process: The precipitation process is carried out at a lower temperature, which can promote the formation of larger crystals and reduce the inclusion of impurities, thereby improving the purity of manganese oxalate. The introduction of ultrasonic treatment during the precipitation process can accelerate the precipitation rate, improve the morphology of the crystals, and may increase the purity of the product;
[0092] Reaction stability: Ensure the stability of the reaction during storage and use to avoid changes in properties caused by long-term storage.
[0093] The specific steps of washing the precipitate are as follows:
[0094] Select appropriate washing solution: Select appropriate washing solution according to the properties of manganese oxalate precipitate to reduce the dissolution loss of manganese oxalate precipitate and avoid the formation of colloid;
[0095] Optimize the number of washing times: Determine the best number of washing times based on the properties of the manganese oxalate precipitate and the required purity. Excessive washing may result in loss of the manganese oxalate precipitate, while too few washing times may not achieve the required purity standard.
[0096] Control the amount of detergent: Adding an appropriate amount of detergent can ensure the washing effect and avoid the loss caused by excessive washing;
[0097] Use appropriate equipment: Use appropriate equipment and tools, including funnels and glass rods, to ensure accuracy and safety of the washing process;
[0098] Vacuum filtration: Use vacuum filtration equipment to separate the precipitate and mother liquor, which can more effectively remove solvents and impurities;
[0099] Repeat washing: After the first washing, it is necessary to repeat washing 3 times to ensure that the impurities on the surface of the manganese oxalate precipitate are thoroughly washed away;
[0100] Drying the manganese oxalate precipitate: After washing, drying the manganese oxalate under vacuum conditions can reduce the drying temperature and prevent thermal decomposition, thereby maintaining the stability and purity of the product for subsequent processing and analysis;
[0101] The above steps all use vacuum treatment to avoid splashing of powder and liquid, making the treatment process more environmentally friendly;
[0102] Recommendations for the drying pellet step:
[0103] Select appropriate drying equipment: According to the properties of manganese oxalate precipitate and experimental requirements, select appropriate drying equipment, including oven and dryer;
[0104] Control drying temperature and time: According to the properties of manganese oxalate precipitate, reasonably set the drying temperature and time to avoid overheating that may cause decomposition or deformation of manganese oxalate precipitate;
[0105] Evenly distribute the manganese oxalate precipitate: Before drying, ensure that the manganese oxalate precipitate is evenly distributed in the container to improve drying efficiency;
[0106] Monitor the drying process: During the drying process, the state of the manganese oxalate precipitate should be checked regularly and the drying parameters should be adjusted in time to ensure the drying effect;
[0107] The specific steps of the post-processing are as follows:
[0108] Choose the right crushing equipment: According to the physical properties of manganese oxalate and the required particle size, choose the most suitable crushing equipment, including hammer crusher, ball mill, and control the particle size and surface modification of the dried manganese oxalate through mechanical grinding, ball milling or other crushing techniques;
[0109] Control the pulverization time: Properly control the pulverization time to avoid the loss of manganese oxalate caused by excessive pulverization, while ensuring that the required particle size can be achieved;
[0110] Screening treatment: Use sieves with different apertures for graded screening to separate manganese oxalate powder that meets specific particle size requirements;
[0111] Optimize the process: Integrate the drying, crushing and screening steps into one continuous process to improve efficiency and reduce costs by reducing manual operations.
[0112] Embodiment 2
[0113] A method for preparing high-purity manganese oxalate, the preparation method is as follows:
[0114] Prepare manganese salt solution: weigh 5 parts of manganese salt (such as manganese sulfate MnSO 4 ·H 2 O), dissolved in deionized water to prepare a manganese salt solution of a certain concentration;
[0115] Prepare oxalic acid solution: weigh 10 parts of oxalic acid (e.g. oxalic acid dihydrate C 2 H2 O 4 ·2H 2 O), dissolved in deionized water to prepare an oxalic acid solution of a certain concentration;
[0116] Mixing reaction: slowly add oxalic acid solution to manganese salt solution, stir at the same time, control the reaction temperature between 60℃, keep the pH value at 7, oxalic acid reacts with manganese salt to form manganese oxalate precipitate;
[0117] Separation of precipitate: When the reaction is complete, let the mixture stand for a while, then separate the manganese oxalate precipitate from the solution by filtration or centrifugation;
[0118] Washing the precipitate: Wash the separated manganese oxalate precipitate with deionized water for 5 times to remove residual ions and impurities;
[0119] Drying the precipitate: drying the washed manganese oxalate precipitate in an oven, or drying it naturally at room temperature until dry manganese oxalate powder is obtained;
[0120] Post-processing: As needed, the dried manganese oxalate is crushed and sieved to obtain a product of the desired particle size.
[0121] The specific steps of preparing the manganese salt solution are as follows:
[0122] Select appropriate manganese salt: According to the requirements of the target product, select appropriate manganese salt, including manganese sulfate and manganese chloride, pre-treat the manganese salt, and remove impurities by heating or filtering to improve the reaction efficiency and the purity of the final product;
[0123] Concentration of solution: According to actual needs, accurately calculate the concentration of manganese salt solution, usually expressed as molar concentration;
[0124] pH value of the solution: Use a buffer solution to control the pH value of the reaction system, so that the required pH environment can be maintained more accurately to facilitate the dissolution of the manganese salt and subsequent reactions;
[0125] Temperature control: Control the temperature of the solution to avoid premature precipitation or decomposition of manganese salts;
[0126] Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration;
[0127] Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
[0128] The specific steps of preparing the oxalic acid solution are as follows:
[0129] Select appropriate oxalic acid: According to actual needs, select appropriate oxalic acid, including oxalic acid dihydrate or anhydrous oxalic acid, pre-treat the oxalic acid, and remove impurities by heating or filtering to improve the reaction efficiency and the purity of the final product;
[0130] Solution concentration: Accurately calculate the concentration of oxalic acid solution according to actual needs, usually expressed in molar concentration;
[0131] pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of oxalic acid and subsequent reactions;
[0132] Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of oxalic acid;
[0133] Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration;
[0134] Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
[0135] The specific steps of the mixed reaction are as follows:
[0136] Choose the right reactants: Choose the right reactants based on the needs of the target product;
[0137] Solution concentration: Accurately calculate the concentration of reactants according to actual needs;
[0138] pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of the reactants and subsequent reactions;
[0139] Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of the reactants;
[0140] Impurity removal: Remove impurities from the solution by appropriate methods such as centrifugation and filtration;
[0141] Precipitation process: The precipitation process is carried out at a lower temperature, which can promote the formation of larger crystals and reduce the inclusion of impurities, thereby improving the purity of manganese oxalate. The introduction of ultrasonic treatment during the precipitation process can accelerate the precipitation rate, improve the morphology of the crystals, and may increase the purity of the product;
[0142] Reaction stability: Ensure the stability of the reaction during storage and use to avoid changes in properties caused by long-term storage.
[0143] The specific steps of washing the precipitate are as follows:
[0144] Select appropriate washing solution: Select appropriate washing solution according to the properties of manganese oxalate precipitate to reduce the dissolution loss of manganese oxalate precipitate and avoid the formation of colloid;
[0145] Optimize the number of washing times: Determine the best number of washing times based on the properties of the manganese oxalate precipitate and the required purity. Excessive washing may result in loss of the manganese oxalate precipitate, while too few washing times may not achieve the required purity standard.
[0146] Control the amount of detergent: Adding an appropriate amount of detergent can ensure the washing effect and avoid the loss caused by excessive washing;
[0147] Use appropriate equipment: Use appropriate equipment and tools, including funnels and glass rods, to ensure accuracy and safety of the washing process;
[0148] Vacuum filtration: Use vacuum filtration equipment to separate the precipitate and mother liquor, which can more effectively remove solvents and impurities;
[0149] Repeat washing: After the first washing, it is necessary to repeat the washing 5 times to ensure that the impurities on the surface of the manganese oxalate precipitate are thoroughly washed away;
[0150] Drying the manganese oxalate precipitate: After washing, drying the manganese oxalate under vacuum conditions can reduce the drying temperature and prevent thermal decomposition, thereby maintaining the stability and purity of the product for subsequent processing and analysis.
[0151] Recommendations for the drying pellet step:
[0152] Select appropriate drying equipment: According to the properties of manganese oxalate precipitate and experimental requirements, select appropriate drying equipment, including oven and dryer;
[0153] Control drying temperature and time: According to the properties of manganese oxalate precipitate, reasonably set the drying temperature and time to avoid overheating that may cause decomposition or deformation of manganese oxalate precipitate;
[0154] Evenly distribute the manganese oxalate precipitate: Before drying, ensure that the manganese oxalate precipitate is evenly distributed in the container to improve drying efficiency;
[0155] Monitor the drying process: During the drying process, the state of the manganese oxalate precipitate should be checked regularly and the drying parameters should be adjusted in time to ensure the drying effect;
[0156] The specific steps of the post-processing are as follows:
[0157] Choose the right crushing equipment: According to the physical properties of manganese oxalate and the required particle size, choose the most suitable crushing equipment, including hammer crusher, ball mill, and control the particle size and surface modification of the dried manganese oxalate through mechanical grinding, ball milling or other crushing techniques;
[0158] Control the pulverization time: Properly control the pulverization time to avoid the loss of manganese oxalate caused by excessive pulverization, while ensuring that the required particle size can be achieved;
[0159] Screening treatment: Use sieves with different apertures for graded screening to separate manganese oxalate powder that meets specific particle size requirements;
[0160] Optimize the process: Integrate the drying, crushing and screening steps into one continuous process to improve efficiency and reduce costs by reducing manual operations.
[0161] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing high-purity manganese oxalate, characterized in that: The preparation method is as follows: Prepare a manganese salt solution: weigh 1-5 parts of manganese salt and dissolve it in deionized water to prepare a manganese salt solution of a certain concentration; Prepare oxalic acid solution: weigh 2-10 parts of oxalic acid and dissolve them in deionized water to prepare an oxalic acid solution of a certain concentration; Mixing reaction: slowly add the oxalic acid solution to the manganese salt solution while stirring, control the reaction temperature between 20-60°C, and keep the pH value within the range of 3-7. Oxalic acid reacts with manganese salt to generate manganese oxalate precipitate; Separation of precipitate: When the reaction is complete, let the mixture stand for a while, then separate the manganese oxalate precipitate from the solution by filtration or centrifugation; Washing the precipitate: Wash the separated manganese oxalate precipitate with deionized water several times to remove residual ions and impurities; Drying the precipitate: drying the washed manganese oxalate precipitate in an oven, or drying it naturally at room temperature until dry manganese oxalate powder is obtained; Post-processing: As needed, the dried manganese oxalate is crushed and sieved to obtain a product of the desired particle size.
2. The method for preparing high-purity manganese oxalate according to claim 1, characterized in that: The specific steps of preparing the manganese salt solution are as follows: Select appropriate manganese salt: According to the requirements of the target product, select appropriate manganese salt, including manganese sulfate and manganese chloride, pre-treat the manganese salt, remove impurities by heating or filtering, and improve the reaction efficiency and purity of the final product; Concentration of solution: According to actual needs, accurately calculate the concentration of manganese salt solution, expressed as molar concentration; pH value of the solution: Use a buffer solution to control the pH value of the reaction system, so as to more accurately maintain the required pH environment to facilitate the dissolution of the manganese salt and subsequent reactions; Temperature control: Control the temperature of the solution to avoid premature precipitation or decomposition of manganese salts; Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration; Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
3. The method for preparing high-purity manganese oxalate according to claim 1, characterized in that: The specific steps of preparing the oxalic acid solution are as follows: Select appropriate oxalic acid: According to actual needs, select appropriate oxalic acid, including oxalic acid dihydrate or anhydrous oxalic acid, pre-treat the oxalic acid, and remove impurities by heating or filtering to improve the reaction efficiency and the purity of the final product; Solution concentration: Accurately calculate the concentration of oxalic acid solution according to actual needs, usually expressed in molar concentration; pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of oxalic acid and subsequent reactions; Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of oxalic acid; Impurity Removal: Remove impurities from the solution by appropriate methods, including centrifugation and filtration; Stability of solution: Ensure the stability of the solution during storage and use to avoid changes in properties caused by long-term storage.
4. The method for preparing high-purity manganese oxalate according to claim 1, characterized in that: The specific steps of the mixed reaction are as follows: Choose the right reactants: Choose the right reactants based on the needs of the target product; Solution concentration: Accurately calculate the concentration of reactants according to actual needs; pH value of the solution: Use a buffer solution instead of directly adjusting the acidity to control the pH value of the reaction system to facilitate the dissolution of the reactants and subsequent reactions; Temperature control: Control the temperature of the solution to avoid premature crystallization or decomposition of the reactants; Impurity removal: Remove impurities from the solution by appropriate methods such as centrifugation and filtration; Precipitation process: Carrying out the precipitation process at a lower temperature promotes the formation of larger crystals and reduces the inclusion of impurities, thereby improving the purity of manganese oxalate. Introducing ultrasonic treatment during the precipitation process can accelerate the precipitation rate, improve the morphology of the crystals, and may increase the purity of the product; Reaction stability: Ensure the stability of the reaction during storage and use to avoid changes in properties caused by long-term storage.
5. The method for preparing high-purity manganese oxalate according to claim 1, characterized in that: The specific steps of washing the precipitate are as follows: Select appropriate washing solution: Select appropriate washing solution according to the properties of manganese oxalate precipitate to reduce the dissolution loss of manganese oxalate precipitate and avoid the formation of colloid; Optimize the number of washing times: Determine the optimal number of washing times based on the properties of the manganese oxalate precipitate and the required purity; Control the amount of detergent: Adding an appropriate amount of detergent can ensure the washing effect and avoid the loss caused by excessive washing; Use appropriate equipment: Use appropriate equipment and tools, including funnels and glass rods, to ensure accuracy and safety of the washing process; Vacuum filtration: Use vacuum filtration equipment to separate the precipitate and mother liquor, which is more effective in removing solvents and impurities; Repeat washing: After the first washing, it is necessary to repeat the washing several times to ensure that the impurities on the surface of the manganese oxalate precipitate are thoroughly washed away; Drying the manganese oxalate precipitate: After washing, the manganese oxalate is dried under vacuum conditions to reduce the drying temperature and prevent thermal decomposition, thereby maintaining the stability and purity of the product for subsequent processing and analysis.
6. The method for preparing high-purity manganese oxalate according to claim 1, characterized in that: Recommendations for the drying pellet step: Select appropriate drying equipment: According to the properties of manganese oxalate precipitate and experimental requirements, select appropriate drying equipment, including oven and dryer; Control the drying temperature and time: According to the properties of the manganese oxalate precipitate, reasonably set the drying temperature and time to avoid overheating that may cause decomposition or deformation of the manganese oxalate precipitate; Evenly distribute the manganese oxalate precipitate: Before drying, ensure that the manganese oxalate precipitate is evenly distributed in the container to improve drying efficiency; Monitor the drying process: During the drying process, the state of the manganese oxalate precipitate should be checked regularly, and the drying parameters should be adjusted in time to ensure the drying effect.
7. The method for preparing high-purity manganese oxalate according to claim 1, characterized in that: The specific steps of the post-processing are as follows: Choose the right crushing equipment: According to the physical properties of manganese oxalate and the required particle size, choose the most suitable crushing equipment, including hammer crusher, ball mill, and control the particle size and surface modification of the dried manganese oxalate through mechanical grinding, ball milling or other crushing techniques; Control the pulverization time: Control the pulverization time to avoid the loss of manganese oxalate due to over-pulverization while ensuring that the required particle size can be achieved; Screening treatment: Use screens with different apertures for graded screening to separate manganese oxalate powder that meets specific particle size requirements; Optimize the process: Integrate the drying, crushing and screening steps into one continuous process to improve efficiency and reduce manual operations to reduce costs.
