CN114737068A - High-efficiency leaching method of high-grade pyrolusite - Google Patents
High-efficiency leaching method of high-grade pyrolusite Download PDFInfo
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- CN114737068A CN114737068A CN202210278364.0A CN202210278364A CN114737068A CN 114737068 A CN114737068 A CN 114737068A CN 202210278364 A CN202210278364 A CN 202210278364A CN 114737068 A CN114737068 A CN 114737068A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B47/00—Obtaining manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention provides a high-efficiency leaching method of high-grade pyrolusite, and relates to the technical field of manganese ore extraction. The high-efficiency leaching method of the high-grade pyrolusite comprises the following steps: firstly, crushing pyrolusite, mixing the crushed pyrolusite with a reducing agent in proportion, and calcining to prepare reduced manganese ore powder; secondly, fully mixing reduced manganese ore powder with pure water according to the solid-to-liquid ratio of 1.0 (1.0-2.0) to prepare slurry; thirdly, adding a certain amount of iron remover into the slurry, and stirring for 10-30 minutes; step four, after stirring for 20 minutes, synchronously adding slurry and concentrated sulfuric acid into the reaction tank at a constant speed, simultaneously supplementing a certain amount of pure water at 50-70 ℃, and maintaining the temperature in the reaction tank at 70-90 ℃; and step five, after reacting for 2 hours, finishing leaching. The leaching operation process of pyrolusite can ensure high leaching rate of manganese, greatly reduce impurity leaching rate, shorten reaction time and has simple requirement on a reactor.
Description
Technical Field
The invention relates to the technical field of extraction of manganese ores, in particular to a high-efficiency leaching method of high-grade pyrolusite.
Background
Pyrolusite is an important raw material for producing manganese series materials. The wet process is the main process for producing the above materials, and the leaching process is an indispensable process in the process. In the wet process for producing manganese-based materials, a sulfuric acid leaching system is basically used. Because MnO2 in the pyrolusite is insoluble in sulfuric acid, MnO2 is converted into MnO by reduction roasting and then can be leached by sulfuric acid, but some impurities of the pyrolusite are easy to leach by sulfuric acid after roasting, especially iron, potassium and the like, so that the pressure and the treatment cost of subsequent purification procedures are increased.
The leaching method of pyrolusite disclosed in patent CN201310736450.2 has high leaching rate and short reaction time; but the reducing agent ammonium sulfite is needed to be used under a closed condition, so that the requirement on the reactor is high and the cost is high; new impurity ammonium ions can be introduced, which is not allowed for the process for producing the battery-grade manganese sulfate product; in addition, the method has high iron ion content in the leachate, and has great influence on the solid-liquid separation in the subsequent neutralization process.
Therefore, the method for leaching pyrolusite by developing the pyrolusite without increasing the burden of the subsequent process has great practical value.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a high-efficiency leaching method of high-grade pyrolusite, and solves the problems of complex conditions and heavy burden in the subsequent processing process of the conventional pyrolusite leaching process.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a high-efficiency leaching method of high-grade pyrolusite comprises the following steps:
firstly, crushing pyrolusite, mixing the crushed pyrolusite with a reducing agent in proportion, and calcining to prepare reduced manganese ore powder;
secondly, fully mixing the reduced manganese ore powder with pure water according to the solid-to-liquid ratio of 1.0 (1.0-2.0) to prepare slurry;
thirdly, adding a certain amount of iron remover into the slurry, and stirring for 10-30 minutes;
fourthly, after stirring for 20 minutes, synchronously adding the slurry and concentrated sulfuric acid into the reaction tank at a constant speed, simultaneously supplementing a certain amount of pure water at 50-70 ℃, and maintaining the temperature in the reaction tank at 70-90 ℃;
and step five, after reacting for 2 hours, finishing leaching.
Preferably, the crushing granularity of pyrolusite after crushing in the first step is required to be-120 meshes and more than 95%.
Preferably, the reducing agent in the first step is a biomass charcoal composite reducing agent.
Preferably, the solid-to-liquid ratio of 1.0 (1.0-2.0) in the second step is the mass ratio of the manganese ore powder of the reduced ore to water.
Preferably, the iron removing agent in the third step is one or a mixture of sodium sulfide, potassium sulfate and ferrous sulfate.
Preferably, the stirring operation time in the third step is 10 to 30 minutes, and the stirring is performed for sufficiently dispersing the iron remover.
Preferably, the synchronous uniform speed in the fourth step means that the manganese ore slurry and the sulfuric acid which are two reaction materials are added in a balanced manner according to a reaction chemical formula.
Preferably, the step four of supplementing pure water with a certain amount of 50-70 ℃ means maintaining the temperature of the system and adjusting the solid-liquid ratio of the reaction.
(III) advantageous effects
The invention provides a high-efficiency leaching method of high-grade pyrolusite. The method has the following beneficial effects:
according to the invention, the leaching operation process of pyrolusite can ensure high leaching rate of manganese, greatly reduce impurity leaching rate, shorten reaction time, has simple requirements on a reactor, has simple leaching conditions, does not introduce excessive impurities during subsequent impurity removal, simplifies impurity removal and leaching steps, and achieves the purpose of efficiently leaching manganese by a simple process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides a high-efficiency leaching method of high-grade pyrolusite, which comprises the following steps:
firstly, crushing pyrolusite, mixing the crushed pyrolusite with a reducing agent in proportion, and calcining the mixture to prepare reduced manganese ore powder;
secondly, fully mixing reduced manganese ore powder with pure water according to a solid-to-liquid ratio of 1.0:1.0-2.0 to prepare pulp, wherein the main purpose of pulp is to fully wet the surface of the ore and improve the mass transfer speed of the subsequent reaction;
thirdly, adding a certain amount of iron remover into the slurry, and stirring for 10 minutes;
fourthly, after stirring for 20 minutes, synchronously adding slurry and concentrated sulfuric acid into the reaction tank at a constant speed, simultaneously supplementing a certain amount of pure water at 50 ℃, and maintaining the temperature in the reaction tank at 70 ℃, wherein the maintenance of the temperature in the reaction tank at 70 ℃ means that in the reaction process, the temperature is in the range of 70 ℃, the manganese leaching rate is highest, and the impurity leaching rate is lowest;
and fifthly, after the reaction is carried out for 2 hours, leaching is finished, and after the reaction is carried out for 2 hours, the leaching rate of manganese reaches the theoretical leaching rate, the leaching operation process of pyrolusite can ensure the high leaching rate of manganese, the impurity leaching rate is greatly reduced, the reaction time is shortened, the requirement on a reactor is simple, the leaching condition is simple, excessive impurities cannot be introduced during subsequent impurity removal, the impurity removal and leaching steps are simplified, and the aim of efficiently leaching manganese by a simple process is fulfilled.
In the first step, the crushed pyrolusite is crushed and the crushed granularity is required to be-120 meshes and more than 95 percent.
The reducing agent in the first step is a biomass charcoal composite reducing agent.
The solid-to-liquid ratio of 1.0:1.0 in the second step is the mass ratio of the manganese ore powder of the reduced ore to water.
The iron removing agent in the third step is one or a mixture of sodium sulfide, potassium sulfate and ferrous sulfate.
The stirring operation time in the third step was 10 minutes, and stirring was used to sufficiently disperse the iron remover.
The synchronous uniform speed in the fourth step means that the manganese ore slurry and the sulfuric acid which are two reaction materials are added in a balanced manner according to a reaction chemical formula.
The addition of a certain amount of pure water of 50 ℃ in the fourth step means maintaining the temperature of the system and adjusting the solid-to-liquid ratio of the reaction.
Example two:
the embodiment of the invention provides a high-efficiency leaching method of high-grade pyrolusite, which comprises the following steps:
step one, 150g of manganese ore powder and 15g of biomass charcoal composite reducing agent are uniformly mixed, roasted at 800 ℃ for 1 hour, cooled and crushed (the granularity is-120 meshes, which is 96.5 percent) for later use;
secondly, weighing 150g of reduced mineral powder, 150mL of pure water and 0.72g of iron remover, adding the weighed materials into a 500mL beaker, stirring the materials for 20 minutes, and heating the materials to 75 ℃;
thirdly, adding 600mL of pure water and 157.5g of 98% concentrated sulfuric acid into 1000mL of the solution, and keeping the temperature at 75 ℃;
step four, simultaneously adding the slurry obtained in the step two and the hot acid obtained in the step three into a 1000mL beaker by adopting a peristaltic pump to ensure that the two reaction raw materials are completely added simultaneously;
fifthly, keeping the reaction temperature at 75 ℃ and sampling and analyzing after 2 hours;
from the result, the leaching rate of manganese is 85.36%, and the iron content in the solution is 1147 mg/L.
Example three:
the embodiment of the invention provides a high-efficiency leaching method of high-grade pyrolusite, which comprises the following steps:
step one, 150g of manganese ore powder and 15g of biomass charcoal composite reducing agent are uniformly mixed, roasted at 800 ℃ for 1 hour, cooled and crushed (the granularity is-120 meshes, which is 96.5 percent) for later use;
secondly, weighing 150g of reduced ore powder, 150mL of pure water and 0.72g of iron remover, adding the materials into a 500mL beaker, stirring for 20 minutes, and heating to 80 ℃;
thirdly, adding 600mL of pure water and 157.5g of 98% concentrated sulfuric acid into 1000mL of the solution, and keeping the temperature at 80 ℃;
step four, simultaneously adding the slurry obtained in the step two and the hot acid obtained in the step three into a 1000mL beaker by adopting a peristaltic pump to ensure that the two reaction raw materials are completely added simultaneously;
fifthly, keeping the reaction temperature at 80 ℃ and sampling and analyzing after 2 hours;
and sixthly, from the result, the leaching rate of manganese is 88.47%, and the content of iron in the solution is 1056 mg/L.
Example four:
the embodiment of the invention provides a high-efficiency leaching method of high-grade pyrolusite, which comprises the following steps:
step one, 150g of manganese ore powder and 15g of biomass charcoal composite reducing agent are uniformly mixed, roasted at 800 ℃ for 1 hour, cooled and crushed (the granularity is-120 meshes, which is 96.5 percent) for later use;
secondly, weighing 150g of reduced mineral powder, 150mL of pure water and 0.72g of iron remover, adding the weighed materials into a 500mL beaker, stirring the materials for 20 minutes, and heating the materials to 85 ℃;
thirdly, adding 600mL of pure water and 157.5g of 98% concentrated sulfuric acid into 1000mL of the solution, and keeping the temperature at 85 ℃;
step four, simultaneously adding the slurry obtained in the step two and the hot acid obtained in the step three into a 1000mL beaker by adopting a peristaltic pump to ensure that the two reaction raw materials are completely added simultaneously;
fifthly, keeping the reaction temperature at 85 ℃ and sampling and analyzing after 2 hours;
and sixthly, from the result, the leaching rate of manganese is 90.71%, and the content of iron in the solution is 973 mg/L.
Example five:
the embodiment of the invention provides a high-efficiency leaching method of high-grade pyrolusite, which comprises the following steps:
step one, 150g of manganese ore powder and 15g of biomass charcoal composite reducing agent are uniformly mixed, roasted at 800 ℃ for 1 hour, cooled and crushed (the granularity is-120 meshes, which is 96.5 percent) for later use;
secondly, weighing 150g of reduced mineral powder, 150mL of pure water and 0.72g of iron remover, adding the weighed materials into a 500mL beaker, stirring the materials for 20 minutes, and heating the materials to 90 ℃;
thirdly, adding 600mL of pure water and 157.5g of 98% concentrated sulfuric acid into 1000mL of the solution, and keeping the temperature at 90 ℃;
step four, simultaneously adding the second-step medium size and the third-step medium hot acid into a 1000mL beaker by adopting a peristaltic pump to ensure that two reaction raw materials are added completely at the same time;
fifthly, keeping the reaction temperature unchanged at 90 ℃, and sampling and analyzing after 2 hours;
and sixthly, from the result, the leaching rate of manganese is 93.46%, and the content of iron in the solution is 827 mg/L.
Example six:
the embodiment of the invention provides a high-efficiency leaching method of high-grade pyrolusite, which comprises the following steps:
step one, 150g of manganese ore powder and 15g of biomass charcoal composite reducing agent are uniformly mixed, roasted at 800 ℃ for 1 hour, cooled and crushed (the granularity is-120 meshes, which is 96.5 percent) for later use;
secondly, weighing 150g of reduced mineral powder, 150mL of pure water and 0.72g of iron remover, adding the weighed materials into a 500mL beaker, stirring the materials for 20 minutes, and heating the materials to 90 ℃;
thirdly, adding 600mL of pure water and 157.5g of 98% concentrated sulfuric acid into 1000mL of the solution, and keeping the temperature at 90 ℃;
step four, simultaneously adding the slurry obtained in the step two and the hot acid obtained in the step three into a 1000mL beaker by adopting a peristaltic pump to ensure that the two reaction raw materials are completely added simultaneously;
fifthly, keeping the reaction temperature unchanged at 90 ℃, and sampling and analyzing after 3 hours;
and in the sixth step, from the result, the leaching rate of manganese is 94.46 percent, and the content of iron in the solution is 753 mg/L.
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 (8)
1. A high-efficiency leaching method of high-grade pyrolusite is characterized by comprising the following steps: the method comprises the following steps:
firstly, crushing pyrolusite, mixing the crushed pyrolusite with a reducing agent in proportion, and calcining to prepare reduced manganese ore powder;
secondly, fully mixing reduced manganese ore powder with pure water according to the solid-to-liquid ratio of 1.0 (1.0-2.0) to prepare slurry;
thirdly, adding a certain amount of iron remover into the slurry, and stirring for 10-30 minutes;
fourthly, after stirring for 20 minutes, synchronously adding the slurry and concentrated sulfuric acid into the reaction tank at a constant speed, simultaneously supplementing a certain amount of pure water at 50-70 ℃, and maintaining the temperature in the reaction tank at 70-90 ℃;
and step five, after reacting for 2 hours, finishing leaching.
2. The efficient leaching method of high-grade pyrolusite according to claim 1, characterized by comprising the following steps: in the first step, the crushed pyrolusite is crushed, and the crushing granularity is required to be-120 meshes and more than 95%.
3. The efficient leaching method of high-grade pyrolusite according to claim 1, characterized by comprising the following steps: the reducing agent in the first step is a biomass charcoal composite reducing agent.
4. The efficient leaching method of high-grade pyrolusite according to claim 1, characterized by comprising the following steps: the solid-liquid ratio in the second step is 1.0 (1.0-2.0) which is the mass ratio of the manganese ore powder of the reduced ore to water.
5. The efficient leaching method of high-grade pyrolusite according to claim 1, characterized by comprising the following steps: the iron removing agent in the third step is one or a mixture of sodium sulfide, potassium sulfate and ferrous sulfate.
6. The efficient leaching method of high-grade pyrolusite according to claim 1, characterized by comprising the following steps: the stirring operation time in the third step is 10-30 minutes, and stirring is used for fully dispersing the iron remover.
7. The efficient leaching method of high-grade pyrolusite according to claim 1, characterized by comprising the following steps: the synchronous uniform speed in the fourth step means that two reaction materials of manganese ore slurry and sulfuric acid are added in a balanced manner according to a reaction chemical formula.
8. The efficient leaching method of high-grade pyrolusite according to claim 1, characterized by comprising the following steps: the step four, supplementing a certain amount of pure water with the temperature of 50-70 ℃ refers to maintaining the temperature of the system and adjusting the solid-liquid ratio of the reaction.
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| WO2020232505A1 (en) * | 2019-05-21 | 2020-11-26 | Mn Energy Limited | Production of manganese sulphate |
| WO2022052670A1 (en) * | 2020-09-09 | 2022-03-17 | 广东邦普循环科技有限公司 | Method for purifying nickel-cobalt-manganese leaching solution |
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2022
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010094161A1 (en) * | 2009-02-18 | 2010-08-26 | 中南大学 | Method for extracting valuable metals from laterite-nickel ore with whole closed-loop circulation of hydrochloric acid |
| CN106119565A (en) * | 2016-06-22 | 2016-11-16 | 湖南大学 | A kind of method that leaching of manganese and silver produce manganese sulfate and silver from manganese-silver ore |
| CN106399724A (en) * | 2016-10-27 | 2017-02-15 | 中南大学 | Microwave reduction roasting and extracting method for manganese oxide ore |
| CN108660326A (en) * | 2018-05-25 | 2018-10-16 | 东北大学 | A method of reduction acidolysis-leaching is simultaneously except iron handles manganese oxide ore |
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| CN110373542A (en) * | 2019-08-29 | 2019-10-25 | 贵州大学 | A kind of method of powdered biomass reduction manganese oxide ore |
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