CN115259230A - Impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching - Google Patents
Impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching Download PDFInfo
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Abstract
The invention provides an impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching, which comprises the following steps: 1) Crushing and uniformly mixing the manganese anode mud, drying to constant weight, uniformly mixing the pretreated manganese anode mud and a mixed flux, and roasting to generate solid-liquid layering; 2) And (3) performing solid-liquid separation, performing water washing on solid-phase sediments for pulping, adding a sulfuric acid solution for reaction, adding a reducing agent, adding ammonia water, adjusting the pH value to 5-7, adding ammonium sulfide, filtering, adding ammonium bicarbonate, filtering to obtain manganese carbonate precipitate and an ammonium sulfate solution, and decomposing into trimanganese tetroxide. The manganous-manganic oxide has higher purity and can be used as a raw material for preparing high-end soft magnetic ferrite.
Description
Technical Field
The invention belongs to the field of industrial waste resource utilization, and particularly relates to an impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching.
Background
In the production process of electrolytic manganese metal, a large amount of anode mud is inevitably generated in an anode area of an electrolytic cell, and 0.05 to 0.08 ton of anode mud is generated for every 1 ton of electrolytic manganese. Manganese in the anode slime mainly exists in the forms of manganese, bivalent manganese, tetravalent manganese and the like, and is a better manganese resource, and main impurities are sulfur, calcium, magnesium, aluminum, silicon, lead, tin, antimony, copper and the like, so that the electrolytic manganese anode slime has complex components. The manganese sulfate is generally used as a pyrolusite raw material in industry, and is produced by adopting an iron powder reduction method, a ferrous sulfate reduction leaching method, a two-ore roasting water leaching method or a two-ore one-step method. However, no matter which method is adopted, because the solid reducing agent is added, the impurity removal difficulty of manganese leaching is high, and the recovery cost is high. Therefore, at present, domestic manufacturers generally use the waste slag as hazardous waste slag stockpiling and steelmaking additive or sell the waste slag at low cost, do not obtain better development and comprehensive utilization, not only waste resources, but also easily cause considerable environmental pollution due to improper treatment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching.
In order to realize the purpose, the invention is realized by the following technical scheme:
an impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching is characterized by comprising the following steps:
1) Crushing and uniformly mixing the manganese anode slime, grinding the manganese anode slime to the grain diameter of less than or equal to 5mm, drying the manganese anode slime to constant weight, uniformly mixing the pretreated manganese anode slime with a mixed flux, roasting the manganese anode slime in a muffle furnace at the temperature of 1020 ℃ for 30-60 in to generate solid-liquid delamination, wherein the solid-liquid delamination is caused by the flux KBF4And an extractant K3AlF6Or Na3AlF6A binary molten salt system;
2) Solid-liquid separation, namely separating liquid-phase fused salt, removing residual fused salt from solid-phase sediment by hydrochloric acid, washing by deionized water, grinding to a particle size of less than 5mm, putting into a reaction kettle with a cooling device, adding a sulfuric acid solution for reaction, and vacuumizing the reaction kettle at normal temperature;
3) Adding a reducing agent, reacting at normal temperature for 5-10 min, adding ammonia water, adjusting the pH value to 5-7, separating and filtering to obtain a manganese sulfate solution; controlling the temperature of the manganese sulfate solution below 50 ℃, adding 1-2 per mill of ammonium sulfide, filtering to further remove heavy metals in the manganese sulfate solution, adding ammonium bicarbonate into the purified manganese sulfate solution, and filtering to obtain manganese carbonate precipitate and an ammonium sulfate solution.
In the scheme, the method comprises the following steps: evaporating and crystallizing an ammonium sulfate solution to prepare high-purity ammonium sulfate, washing a manganese carbonate precipitate by deionized water, calcining for 1-3 s at 800-900 ℃ by adopting a suspension low-temperature instantaneous firing system, decomposing to obtain trimanganese tetroxide, crushing or sanding solid trimanganese tetroxide, washing by the deionized water, and drying to obtain the finished trimanganese tetroxide.
In the scheme, the method comprises the following steps: the mass ratio of the pretreated electrolytic manganese anode mud to the mixed flux is 1.
In the scheme, the method comprises the following steps: adding sulfuric acid solution according to the content of manganese dioxide, wherein the dosage of the sulfuric acid is 1.5-2 times of the theoretical amount, and the concentration of the sulfuric acid solution is 400g/L.
In the scheme, the method comprises the following steps: the reducing agent is 1,3, 5-triaminobenzene or aminophenol.
In the scheme, the method comprises the following steps: the aminophenol is any one of o-aminophenol, m-aminophenol and p-aminophenol.
In the scheme, the method comprises the following steps: adding a reducing agent according to the content of the manganese dioxide, wherein the dosage of the reducing agent is 1.5-2 times of the theoretical amount.
The impurities of silicon and aluminum in the manganese anode mud are very stable in the structures of formed aluminate and silicate and are very difficult to remove under the acidic condition. Fluxing agent KBF in mixed flux4Melting started at 530 ℃ and KBF increased with increasing temperature to 1020 ℃4KF and BF produced by decomposition3In which gaseous BF is3Volatilisation and the KF disassociates in the molten salt to produce K+And F-Wherein, K is+The manganese anode mud has strong permeability and corrosivity, F-has strong fluidity and corrosivity, and the two synergistically act to destroy the mineral structure of the manganese anode mud, so that manganese ions and other impurity ions are released. Na (Na)3AlF6Or K3AlF6Impurities such as silicon, aluminum and the like can be selectively extracted into liquid-phase molten salt in a molten state, and metals such as manganese, lead, tin, copper, calcium, magnesium and the like in the manganese anode slime exist in a lower layer of the molten salt in a solid-phase deposit mode. Therefore, on one hand, the technology destroys the mineral structure of the manganese anode slime, and releases manganese elements; on the other hand, impurity elements such as silicon, aluminum and the like are removed in the solid-liquid separation of the molten salt for preparing the trimanganese tetroxide for the soft magnet.
After solid-liquid separation (pouring out the upper liquid phase molten salt), mn in the solid phase sediment is treated by 1,3, 5-triaminobenzene or aminophenol4+Reduction of Mn2+Then, compared with the prior art which adopts reducing agents such as diamine, diphenol and the like, the reducing groups of the 1,3, 5-triaminobenzene and aminophenol are more, the reducing performance is stronger, the reducing process is shortened, and the Mn is improved2+The conversion rate of (2). Adding sulfuric acid to add Mn2+Converting into manganese sulfate, reacting calcium, magnesium, lead and sulfuric acid to exist in the form of sulfate precipitates, enabling impurity elements such as tin, antimony, titanium, copper and the like to still exist in the solution in the form of sulfate, adjusting the pH value of the solution to be 5-7 by using ammonia water, enabling impurity elements such as tin, antimony, titanium, copper and the like to exist in the form of hydroxide precipitates, and filtering out impurities such as calcium, magnesium, lead, tin, antimony, titanium, copper and the like. Manganese exists in the filtrate in the form of manganese sulfate, ammonium sulfide is added to precipitate heavy metal so as to further remove heavy metal impurities of manganese sulfate, and extraction is carried outThe purity of manganese sulfate is high.
Has the beneficial effects that:
(1) By adopting the technical scheme, the recovery rate of extracting and recovering manganese from the manganese anode slime can reach more than 99.3% by utilizing the molten salt and acid leaching for impurity removal.
(2) By adopting the technical scheme, the 1,3, 5-triaminobenzene or aminophenol is used for normal temperature reduction, the reduction efficiency is higher than that of the prior art, the reduction time is shortened, and the process of producing high-purity trimanganese tetroxide from manganese anode mud is accelerated.
(3) By adopting the technical scheme, compared with the prior art, the impurity removal is more thorough, the purity of the obtained manganous-manganic oxide is higher, the manganous-manganic oxide can be used as a raw material for preparing high-end soft magnetic ferrite, and the problems of resource waste and environmental pollution caused by manganese anode slime of electrolytic manganese manufacturers are solved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Crushing the manganese anode mud, uniformly mixing, grinding until the particle size is less than or equal to 5mm, and drying in an oven at the temperature of 110 ℃ to constant weight. Uniformly mixing the dried manganese anode mud and a mixed flux according to the proportion of 14And K3AlF6The binary molten salt system consists of 40 percent by mass and 60 percent by mass. Roasting in a muffle furnace at 1020 ℃ for 30-60 min to generate solid-liquid delamination. Removing a molten salt phase after solid-liquid separation, removing residual molten salt from solid-phase sediment by using hydrochloric acid, washing by using deionized water, grinding to be less than 5mm, placing into a reaction kettle with a cooling device, adding 400g/L of sulfuric acid solution according to the content of manganese dioxide in the solid-phase sediment, wherein the dosage of the sulfuric acid is 1.6 times of the theoretical amount, vacuumizing the reaction kettle at normal temperature, adding 1,3, 5-triaminobenzene, adding the reducing agent according to the content of the manganese dioxide, and adding the reducing agent in an amount which is 2 times of the theoretical amount. After reacting for 5-10 min, adding ammonia water, adjusting the pH value to 5-7, and separating and filtering through a filter press to obtain a manganese sulfate solution. Controlling the temperature of the manganese sulfate solution below 50 ℃, adding 2 per mill of ammonium sulfide, filtering to further remove heavy metals in the manganese sulfate solution,and adding ammonium bicarbonate into the purified manganese sulfate solution according to the amount of manganese dioxide, wherein the amount of the ammonium bicarbonate is 2 times of the theoretical amount, and filtering to obtain a manganese carbonate precipitate and an ammonium sulfate solution. Evaporating and crystallizing an ammonium sulfate solution to prepare high-purity ammonium sulfate, washing a manganese carbonate precipitate by deionized water, calcining for 1-3 s at 800-900 ℃ by using a suspension low-temperature instantaneous firing system (ZL 201110100752.1), decomposing to obtain solid trimanganese tetroxide, crushing or sanding the solid trimanganese tetroxide, washing by the deionized water, and drying to obtain a finished product trimanganese tetroxide, wherein the recovery rate is 99.3 percent, and the purity is more than 99.5 percent.
Example 2
Crushing the manganese anode mud, uniformly mixing the crushed manganese anode mud with the particle size of less than or equal to 5mm, and drying the manganese anode mud in an oven at the temperature of 110 ℃ to constant weight. Uniformly mixing the dried manganese anode mud and a mixed flux according to the proportion of 14And Na3AlF6The binary molten salt system consists of 40 percent by mass and 60 percent by mass. Roasting in a muffle furnace at 1020 ℃ for 30-60 min to generate solid-liquid delamination. And (2) discarding a molten salt phase after solid-liquid separation, removing residual molten salt from the solid-phase sediment by hydrochloric acid, washing with deionized water, grinding to below 5mm, placing into a reaction kettle with a cooling device, adding 400g/L sulfuric acid solution according to the content of manganese dioxide in the solid-phase sediment, wherein the dosage of sulfuric acid is 1.5 times of the theoretical amount, vacuumizing the reaction kettle at normal temperature, adding a reducing agent o-aminophenol, adding the reducing agent according to the content of manganese dioxide, and adding the reducing agent in an amount of 1.5 times of the theoretical amount. After reacting for 5-10 min, adding ammonia water, adjusting the pH value to 5-7, and separating and filtering through a filter press to obtain a manganese sulfate solution. Controlling the temperature of the manganese sulfate solution to be below 50 ℃, adding 1 per mill of ammonium sulfide, filtering to further remove heavy metals in the manganese sulfate solution, adding ammonium bicarbonate into the purified manganese sulfate solution according to the amount of manganese dioxide, wherein the amount of ammonium bicarbonate is 1.5 times of the theoretical amount, and filtering to obtain manganese carbonate precipitate and an ammonium sulfate solution. Evaporating and crystallizing an ammonium sulfate solution to prepare high-purity ammonium sulfate, washing manganese carbonate precipitate by deionized water, calcining for 1-3 s at 800-900 ℃ by adopting a suspension low-temperature instantaneous firing system (ZL 201110100752.1), and decomposing to obtain solid tetraoxideAnd (3) manganomanganic, namely crushing or sanding the solid manganomanganic oxide, washing with deionized water, and drying to obtain a finished product of manganomanganic oxide, wherein the recovery rate is 99.4 percent, and the purity is more than 99.5 percent.
Example 3
The manganese anode slime is crushed and then evenly mixed, the particle size is less than or equal to 5mm, and the manganese anode slime is dried to constant weight in an oven at the temperature of 110 ℃. Uniformly mixing the dried manganese anode mud and a mixed flux according to the proportion of 14And Na3AlF6The binary molten salt system consists of 40 percent by mass and 60 percent by mass. Roasting in a muffle furnace at 1020 ℃ for 30-60 min to generate solid-liquid delamination. Removing a molten salt phase after solid-liquid separation, removing residual molten salt from solid-phase sediment by using hydrochloric acid, washing by using deionized water, grinding to be less than 5mm, placing into a reaction kettle with a cooling device, adding 400g/L sulfuric acid solution according to the content of manganese dioxide in the solid-phase sediment, wherein the dosage of the sulfuric acid is 2 times of the theoretical amount, vacuumizing the reaction kettle under the normal temperature condition, adding reducing agent m-aminophenol, adding the reducing agent according to the content of the manganese dioxide, and adding the reducing agent in an amount which is 1.5 times of the theoretical amount. After reacting for 5-10 min, adding ammonia water, adjusting the pH value to 5-7, and separating and filtering through a filter press to obtain a manganese sulfate solution. Controlling the temperature of the manganese sulfate solution to be below 50 ℃, adding 1 per mill of ammonium sulfide, filtering to further remove heavy metals in the manganese sulfate solution, adding ammonium bicarbonate into the purified manganese sulfate solution according to the amount of manganese dioxide, wherein the amount of ammonium bicarbonate is 1.2 times of the theoretical amount, and filtering to obtain manganese carbonate precipitate and an ammonium sulfate solution. Evaporating and crystallizing an ammonium sulfate solution to prepare high-purity ammonium sulfate, washing a manganese carbonate precipitate by deionized water, calcining for 1-3 s at 800-900 ℃ by adopting a suspension low-temperature instantaneous firing system (ZL 201110100752.1), decomposing to obtain solid trimanganese tetroxide, crushing or sanding the solid trimanganese tetroxide, washing by the deionized water, and drying to obtain a finished product trimanganese tetroxide, wherein the recovery rate is 99.2%, and the purity is more than 99.5%.
Example 4
The manganese anode slime is crushed and then evenly mixed, the particle size is less than or equal to 5mm, and the manganese anode slime is dried to constant weight in an oven at the temperature of 110 ℃. Mixing the dried manganese anode mud with a mixed flux14And K3AlF6The binary molten salt system consists of 40 percent by mass and 60 percent by mass. Roasting in a muffle furnace at 1020 ℃ for 30-60 min to generate solid-liquid delamination. And (2) discarding a molten salt phase after solid-liquid separation, washing the solid-phase sediment to prepare pulp, grinding the pulp to be less than 5mm, putting the pulp into a reaction kettle with a cooling device, adding 400g/L of sulfuric acid solution according to the content of manganese dioxide in the solid-phase sediment, wherein the dosage of sulfuric acid is 1.5 times of the theoretical amount, vacuumizing the reaction kettle at normal temperature, adding a reducing agent p-aminophenol, adding the reducing agent according to the content of manganese dioxide, and adding the reducing agent in an amount which is 1.5 times of the theoretical amount. After reacting for 5-10 min, adding ammonia water, adjusting the pH value to 5-7, and separating and filtering through a filter press to obtain a manganese sulfate solution. Controlling the temperature of the manganese sulfate solution to be below 50 ℃, adding 1 per mill of ammonium sulfide, filtering to further remove heavy metals in the manganese sulfate solution, adding ammonium bicarbonate into the purified manganese sulfate solution according to the amount of manganese dioxide, wherein the amount of the ammonium bicarbonate is 1.2 times of the theoretical amount, and filtering to obtain manganese carbonate precipitate and an ammonium sulfate solution. Evaporating and crystallizing an ammonium sulfate solution to prepare high-purity ammonium sulfate, washing a manganese carbonate precipitate by deionized water, calcining for 1-3 s at 800-900 ℃ by adopting a suspension low-temperature instantaneous firing system (ZL 201110100752.1), decomposing to obtain solid trimanganese tetroxide, crushing or sanding the solid trimanganese tetroxide, washing by the deionized water, and drying to obtain a finished product trimanganese tetroxide, wherein the recovery rate is 99.3%, and the purity is more than 99.5%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. An impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching is characterized by comprising the following steps:
1) Crushing the manganese anode mud, uniformly mixing, and grinding to particlesThe diameter is less than or equal to 5mm, the mixture is dried to constant weight, the pretreated manganese anode mud and the mixed flux are uniformly mixed, and the mixture is roasted in a muffle furnace at 1020 ℃ for 30-60 min to generate solid-liquid stratification, namely the flux KBF4And an extractant K3AlF6Or Na3AlF6A binary molten salt system;
2) Separating solid and liquid, separating liquid phase molten salt, removing residual molten salt from solid phase sediment by hydrochloric acid, washing with deionized water, grinding to particle size below 5mm, placing into a reaction kettle with a cooling device, adding sulfuric acid solution for reaction, and vacuumizing the reaction kettle at normal temperature;
3) Adding a reducing agent, reacting at normal temperature for 5-10 min, adding ammonia water, adjusting the pH value to 5-7, separating and filtering to obtain a manganese sulfate solution; controlling the temperature of the manganese sulfate solution below 50 ℃, adding 1-2 per mill of ammonium sulfide, filtering to further remove heavy metals in the manganese sulfate solution, adding ammonium bicarbonate into the purified manganese sulfate solution, and filtering to obtain manganese carbonate precipitate and an ammonium sulfate solution.
2. The impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by using molten acid leaching according to claim 1, is characterized in that: evaporating and crystallizing an ammonium sulfate solution to prepare high-purity ammonium sulfate, washing a manganese carbonate precipitate by deionized water, calcining for 1-3 s at 800-900 ℃ by adopting a suspension low-temperature instantaneous firing system, decomposing to obtain trimanganese tetroxide, crushing or sanding solid trimanganese tetroxide, washing by the deionized water, and drying to obtain the finished trimanganese tetroxide.
3. The method for removing impurities in the production of trimanganese tetroxide for soft magnetic materials from electrolytic manganese anode slime by molten acid leaching according to claim 1, wherein the method comprises the following steps: the mass ratio of the pretreated electrolytic manganese anode mud to the mixed flux is 1.
4. The method for removing impurities in the production of trimanganese tetroxide for soft magnetic materials from electrolytic manganese anode slime by molten acid leaching according to claim 2, wherein the method comprises the following steps: adding sulfuric acid solution according to the content of manganese dioxide, wherein the dosage of the sulfuric acid is 1.5-2 times of the theoretical amount, and the concentration of the sulfuric acid solution is 400g/L.
5. The method for removing impurities in the production of trimanganese tetroxide for soft magnetism from electrolytic manganese anode slime by using molten acid leaching according to claim 4, wherein the method comprises the following steps: the reducing agent is 1,3, 5-triaminobenzene or aminophenol.
6. The impurity removing method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by using molten acid leaching according to claim 5, wherein the method comprises the following steps: the aminophenol is any one of o-aminophenol, m-aminophenol and p-aminophenol.
7. The method for removing impurities in the production of trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by using molten acid leaching according to claim 6, wherein the method comprises the following steps: adding a reducing agent according to the content of manganese dioxide, wherein the dosage of the reducing agent is 1.5-2 times of the theoretical quantity.
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| CN116621225A (en) * | 2023-07-12 | 2023-08-22 | 重庆上甲电子股份有限公司 | Flux and method for recovering manganese from perillaldehyde waste residues and application of flux and method for preparing trimanganese tetroxide for soft magnetism |
| CN116654988A (en) * | 2023-07-12 | 2023-08-29 | 重庆大学 | Method for preparing battery grade manganous-manganic oxide by using manganese-containing waste residues |
| CN116835971A (en) * | 2023-07-12 | 2023-10-03 | 华东师范大学 | Method for preparing high saturation magnetic induction density manganese-zinc ferrite material by using manganese waste residues and zinc waste residues |
| CN116875827A (en) * | 2023-07-12 | 2023-10-13 | 重庆上甲电子股份有限公司 | Method for preparing soft magnetic manganese zinc ferrite composite material by utilizing manganese-containing waste residues and zinc-containing waste residues generated in production of perillaldehyde |
| CN116621225B (en) * | 2023-07-12 | 2024-01-23 | 重庆上甲电子股份有限公司 | Flux and method for recovering manganese from perillaldehyde waste residues and application of flux and method for preparing trimanganese tetroxide for soft magnetism |
| CN116835971B (en) * | 2023-07-12 | 2024-02-27 | 华东师范大学 | Method for preparing high saturation magnetic induction density manganese-zinc ferrite material by using manganese waste residues and zinc waste residues |
| CN116875827B (en) * | 2023-07-12 | 2024-03-15 | 重庆上甲电子股份有限公司 | Method for preparing soft magnetic manganese zinc ferrite composite material by utilizing manganese-containing waste residues and zinc-containing waste residues generated in production of perillaldehyde |
| CN116654988B (en) * | 2023-07-12 | 2024-03-19 | 重庆大学 | Method for preparing battery grade manganous-manganic oxide by using manganese-containing waste residues |
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| CN115259230B (en) | 2023-04-18 |
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