CN108085486A - A kind of method for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method - Google Patents
A kind of method for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method Download PDFInfo
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- CN108085486A CN108085486A CN201810029181.9A CN201810029181A CN108085486A CN 108085486 A CN108085486 A CN 108085486A CN 201810029181 A CN201810029181 A CN 201810029181A CN 108085486 A CN108085486 A CN 108085486A
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- pyrolusite
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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
- 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
- C22B47/00—Obtaining manganese
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Abstract
The invention discloses a kind of method that manganese is extracted from low-grade pyrolusite with grinding pressurization combination method, including step：（1）Dry pyrolusite is formed into pyrolusite powder after substep is ground；（2）By lignite with 0.5 mol L‑1Re-dry after sulfuric acid solution forms lignite powder after substep is ground；（3）Above-mentioned pyrolusite powder with lignite powder is mixed, and is fully ground, forms pyrolusite/lignite compound；（4）By above-mentioned pyrolusite/lignite compound in nitrogen atmosphere, 200OC~550OA period of time is kept the temperature under C, is cooled to room temperature, obtains preconditioning compound；（5）By above-mentioned preconditioning compound and 1 mol L‑1The mixture of sulfuric acid solution be transferred in autoclave, 180OC~300 OCertain time is kept under C, gained filtrate is pyrolusite extracting solution, and gained filter residue can use after drying as fuel.The cost of material of the present invention is low, and reaction process is simple, and the extraction rate of manganese is high, is suitable for the extraction process of industrial pyrolusite.
Description
Technical field
The present invention relates to one kind using lignite as reducing agent, by grinding-pressurization integrated processes, soaked from low-grade pyrolusite
The technique for going out manganese, belongs to field of hydrometallurgy.
Background technology
Manganese product in daily life and has highly important effect in industrial and agricultural production.At present, manganese product
Alloy field is mainly used in, and manganese dioxide is then mainly used in one-shot battery and secondary battery industry, is widely used
It is general.The most common mineral of manganese are pyrolusites, and main component is manganese dioxide, and manganese is also deposited in the form of some other mineral
, such as manganese spar (MnCO3), rhodonite (MnSiO3), hausmannite (MnOOH), alabandite (MnS) etc..China's manganese ore money
Source is mainly distributed on the ground such as Guangxi, Hunan, Yunnan, Guizhou, and the quality and its grade of ore are poor compared with external, how to develop
Manganese resource using China is that national economy service is an important problem.
Low-grade pyrolusite (Mn%<40%) it is relatively more in the west and south in China, but manganese therein how is extracted, particularly
Reducing process this key technical problem how is solved, is still the important step of pyrolusite utilization.In pyrolusite manganese from
Son mainly exists in the form of manganese dioxide, and high price manganese dioxide is reduced to low price manganese () by reducing agent, then in acyclic acidic
Be changed into border soluble manganese salt by manganese the reducing leaching from ore.
At present, the main method for extracting manganese from pyrolusite has：
（1）High-temperature roasting reduction method：This is the conventional method for preparing manganese sulfate product, is 700-900 DEG C in reduction roasting temperature
Under, manganese dioxide is finally reduced to divalent manganese oxide in pyrolusite, so as to extract manganese in an acidic solution.In reduction process
The reducing substanceses such as reducing agent generally use coal dust, carbon monoxide, hydrogen, methane.The method reduction process will use reverberatory furnace,
The equipment such as reduction furnace, rotary kiln, and cooling water is also sprayed after high-temperature roasting is quickly cooled down rotary kiln, otherwise, the oxidation of generation
Manganese can be oxidized to manganese sesquioxide managnic oxide in air.The manganese oxide of generation is basic anhydride, it is easy to be occurred with dilute sulfuric acid anti-
Is answered in addition, the major defect of the method is to consume the substantial amounts of energy, pollution is big, is unfavorable for the development of pyrolusite.
（2）Sulfur dioxide reduction method：Although sulphur dioxide reduction pyrolusite technics comparing is ripe, there is dithionate
Generation, influence the quality of product, up to the present also industrially large-scale application, is only applied in environmental protection
Desulfurization.
（3）Two ore deposit one-step method：This is the more reducing leaching reaction of research, this reaction not only can will be in pyrolusite
Manganese dioxide reducing leaching, but also ferrous disulfide in pyrite can be changed into ferric sulfate.Two ore deposit one-step method can be anti-
A step in slot is answered to complete, technological process is simple, and pyrite is resourceful, can meet the needs of pyrolusite reduction, to a certain extent
Improve the environment of operation.But manganese leaching rate is low, cleans and purifies the requirement that electrolytic manganese parameter is not achieved, fail in electricity
It is realized in solution manganese and manganese dioxide technique.In addition, the method can also generate substantial amounts of waste residue, subsequent processing is cumbersome.
（4）Organic matter reduction method：Using the organic matters conduct such as glucose, sucrose, lactose, crop products or byproduct
Reducing agent can react with the manganese dioxide in pyrolusite in sour environment, value Mn is reduced to Mn2+.This side
Method reaction temperature is moderate, and cost of investment is low, is a kind of feasible route.But organic matter as reducing agent when Leach reaction not
It is enough thorough, a small amount of small molecule can be generated and be dissolved in leachate, it is clean to be not easy purification, particularly in electrolytic industry, a small amount of
Organic matter, which this may result in electrolysis, to be normally carried out.
（5）Hydrogen peroxide reduction method：When making reducing agent with hydrogen peroxide, more hydrogen peroxide is consumed, the higher price of the latter,
Significantly increase the cost of whole process.
（6）Biological reducing method：When making reducing agent using microorganism, the manganese in pyrolusite can also be soaked with higher efficiency
Go out.But for leaching after the completion of, how microorganism is handled, and how leachate purifies and finally obtain pure manganese product also not
It is resolved.
（7）Ferrous ion or iron filings lixiviation process：Using the reproducibility of ferrous ion in an acidic solution, by pyrolusite with compared with
Fast speed is reduced to soluble manganese ion, and here it is the basic principles of ferrous ion reduction method.In acid pyrolusite solution,
Sponge iron is directly added into, the tetravalent manganese in pyrolusite can be made promptly to be reduced into divalent violent, it is more more efficient than with ferrous sulfate.
Both approaches are inherently essentially identical, but in their subsequent processes, substantial amounts of iron hydroxide is separated
It removes, there are process is complicated, impurity level is more, the problems such as difficult.
Lignite also known as bavin coal are the minimum pit coals of degree of coalification.It is a kind of dark brown between peat and pitch coal
Color, lacklustre rudimentary coal.Its chemical reactivity is strong, has stronger reproducibility.But since the degree of coalification of lignite is low, institute
It is not excellent bunker coal with it.However, exactly because its degree of coalification is low, wherein organising containing largely oxidable
Object is closed, therefore, pyrolusite is reduced using it as reducing agent, is feasible so as to extract manganese, from the comprehensive utilization of lignite
With important practical significance.
The present invention, in an acidic solution, will be in pyrolusite by improving reaction temperature and pressure using lignite as reducing agent
Value Mn be reduced to soluble bivalent manganese, so as to fulfill low cost, the process of high efficiency extraction manganese.Due to this be solid-solid-
Reaction between liquid, so lignite and pyrolusite particle are fully ground powdering particle by the present invention respectively first；Then by this
Two kinds of solid particles mix, then are fully ground, since they are the particles of nano particle grade, in such high speed grinding
Under, both particles can be contacted sufficiently, so as to be very beneficial for their subsequent reactions.Then by them in sulfuric acid solution
Middle carry out ultrasonic disperse；It is finally fully reacted in hydrothermal reaction kettle again, manganese reduction, the leaching in pyrolusite is come out, filtered
Slag can use after drying as fuel.Cost of material of the present invention is low, and reaction process is simple, and the reaction time contracts significantly
Short, the extraction rate of manganese is high, is suitable for the extraction process of industrial pyrolusite.
The content of the invention
The object of the present invention is to provide a kind of methods for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method.
Embodiment of the present invention is：A kind of method for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method,
Comprise the following steps：
（1）First by pyrolusite solid 80ODried pyrolusite beforehand research is then worn into particle by the air drying of C, then
The pyrolusite particle of this pre-grinding is continued to be ground into pyrolusite powder；
（2）By lignite and 0.5 mol L-1Sulfuric acid solution mixes, 50OIt heats and is sufficiently stirred in C water-baths, filter, washing, institute
Lignite is obtained 80OThe progress beforehand research of dried lignite is then worn into particle by the air drying of C, then by this pre-grinding
Lignite particle continues to be ground into lignite powder；
（3）The pyrolusite powder that above-mentioned grain size is 500 nm or so is mixed with the lignite powder that grain size is 300 nm or so, and
It is fully ground, forms pyrolusite/lignite compound；The pyrolusite powder that the grain size is 500 nm or so and grain size are 300 nm
The mass ratio of the lignite powder of left and right is 1: 1 ~ 5；
（4）By above-mentioned pyrolusite/lignite compound in nitrogen atmosphere, with 4OC min-1Speed be heated to 200OC ~
550OC, and heat preservation a period of time, subsequent cooled to room temperature obtain preconditioning compound at this temperature；
（5）By above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution mixing, the mixture is then transferred to reaction under high pressure
180 are heated in kettleOC ~ 300 OC simultaneously keeps certain time, is subsequently cooled to room temperature, and filtering, gained filtrate is pyrolusite
Then extracting solution extracts violent from pyrolusite extracting solution；The quality of the preconditioning compound and 1 mol L-1Sulfuric acid solution
The ratio between quality volume be 15 ~ 50 g: 100mL.
Preferably, step（1）In, by dried pyrolusite pre-grinding into the particle that grain size is 1 mm or so, then will
The pyrolusite particle of this pre-grinding continues to be ground into pyrolusite powder of the grain size for 500 nm or so.
Preferably, step（2）In, it is the particle of 1 mm or so by dried lignite pre-grinding, then by this beforehand research
The lignite particle of mill continues to be ground into lignite powder of the grain size for 300 nm or so.
Preferably, step（4）In, the heating temperature is 350OC ~450OC, optimum temperature 400 OC。
Preferably, step（5）In, the heating temperature is 250OC 。
The present invention forms the very big little particle of surface area, so as to ensure soft manganese by the way that pyrolusite and lignite are fully ground
Ore deposit has sufficient contact area with both solid matters of lignite in reaction；By by the pyrolusite after being fully ground and lignite
Mixing, and further grind, come into full contact with the particle of the two；Further this hybrid solid object is added at a certain temperature
Heat, since pyrolusite and lignite come into full contact with so that value Mn in pyrolusite can partial reduction be low price manganese；Again finally
It is reacted by high temperature, high-pressure leaching, comes out the leaching completely of the value Mn in pyrolusite, and the filter residue of gained is not predominantly anti-
Should or the smaller lignite of the extent of reaction, can be used after drying as fuel.The cost of material of the present invention is low, reaction process letter
Single, the extraction rate of manganese is high, is suitable for the extraction process of industrial pyrolusite.
Inventive embodiments
Embodiment 1：
（1）First by pyrolusite solid 80OWhen drying 24 is small in the air drying cabinet of C；Then dried pyrolusite is put
Pre-grinding is carried out in general milling machine, is ground into particle of the grain size for 1 mm or so；Again by the soft manganese of this pre-grinding
Ore deposit particle is transferred in high speed ball mill, it is continued to be ground into pyrolusite powder of the grain size for 500 nm or so.
（2）By lignite and 0.5 mol L-1Sulfuric acid solution mixes, 50OHeated in C water-baths and stir 3 it is small when；Subsequent mistake
Filter, is washed with water twice, gained lignite is 80OWhen drying 24 is small in the air drying cabinet of C；Then dried lignite is placed in general
Pre-grinding is carried out in logical ball mill, is ground into particle of the grain size for 1 mm or so；Again by the lignite particle of this pre-grinding
It is transferred in high speed ball mill, it is continued to be ground into lignite powder of the grain size for 300 nm or so.
（3）It is the lignite powder of 300 nm or so by 1 by pyrolusite powder that above-mentioned grain size is 500 nm or so and grain size:
1 mass ratio, which is placed in high speed ball mill, to be mixed, and be fully ground 0.5 ~ 1.5 it is small when, formed pyrolusite/lignite compound.
（4）Above-mentioned pyrolusite/lignite compound is transferred in tube furnace, in nitrogen atmosphere, with 4OC min-1Speed
It is heated to 200OC, and at this temperature keep 2 it is small when, subsequent cooled to room temperature obtains preconditioning compound；
（5）By above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution press 15:The ratio mixing of 100mL, then mixes this
It closes object to be transferred in autoclave, is heated to 180OWhen C temperature and small holding 4；Room temperature is then cooled to, is filtered, filter residue is used
Neutrality is washed to, the filter residue of gained can use after drying as fuel；Gained filtrate is pyrolusite extracting solution, wherein solvable
The Mn of property2+Content analyzed using conventional atomic absorption spectroscopy, the extraction efficiency for obtaining manganese in pyrolusite is
93%。
Embodiment 2：
（1）First by pyrolusite solid 80OWhen drying 24 is small in the air drying cabinet of C；Then dried pyrolusite is put
Pre-grinding is carried out in general milling machine, is ground into particle of the grain size for 1 mm or so；Again by the soft manganese of this pre-grinding
Ore deposit particle is transferred in high speed ball mill, it is continued to be ground into pyrolusite powder of the grain size for 500 nm or so.
（2）By lignite and 0.5 mol L-1Sulfuric acid solution mixes, 50OHeated in C water-baths and stir 3 it is small when；Subsequent mistake
Filter, is washed with water twice, gained lignite is 80OWhen drying 24 is small in the air drying cabinet of C；Then dried lignite is placed in general
Pre-grinding is carried out in logical ball mill, is ground into particle of the grain size for 1 mm or so；Again by the lignite particle of this pre-grinding
It is transferred in high speed ball mill, it is continued to be ground into lignite powder of the grain size for 300 nm or so.
（3）It is the lignite powder of 300 nm or so by 1 by pyrolusite powder that above-mentioned grain size is 500 nm or so and grain size:
2 mass ratio, which is placed in high speed ball mill, to be mixed, and be fully ground 1 it is small when, formed pyrolusite/lignite compound.
（4）Above-mentioned pyrolusite/lignite compound is transferred in tube furnace, in nitrogen atmosphere, with 4OC min-1Speed
It is heated to 300OC, and at this temperature keep 2 it is small when, subsequent cooled to room temperature obtains preconditioning compound；
（5）By above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution press 30:The ratio mixing of 100mL, then mixes this
It closes object to be transferred in autoclave, is heated to 240OWhen C temperature and small holding 2；Room temperature is then cooled to, is filtered, filter residue is used
Neutrality is washed to, the filter residue of gained can use after drying as fuel；Gained filtrate is pyrolusite extracting solution, wherein solvable
The Mn of property2+Content analyzed using conventional atomic absorption spectroscopy, the extraction efficiency for obtaining manganese in pyrolusite is
96%。
Embodiment 3：
（1）First by pyrolusite solid 80OWhen drying 24 is small in the air drying cabinet of C；Then dried pyrolusite is put
Pre-grinding is carried out in general milling machine, is ground into particle of the grain size for 1 mm or so；Again by the soft manganese of this pre-grinding
Ore deposit particle is transferred in high speed ball mill, it is continued to be ground into pyrolusite powder of the grain size for 500 nm or so.
（2）By lignite and 0.5 mol L-1Sulfuric acid solution mixes, 50OHeated in C water-baths and stir 3 it is small when；Subsequent mistake
Filter, is washed with water twice, gained lignite is 80OWhen drying 24 is small in the air drying cabinet of C；Then dried lignite is placed in general
Pre-grinding is carried out in logical ball mill, is ground into particle of the grain size for 1 mm or so；Again by the lignite particle of this pre-grinding
It is transferred in high speed ball mill, it is continued to be ground into lignite powder of the grain size for 300 nm or so.
（3）It is the lignite powder of 300 nm or so by 1 by pyrolusite powder that above-mentioned grain size is 500 nm or so and grain size:
5 mass ratio, which is placed in high speed ball mill, to be mixed, and be fully ground 1.5 it is small when, formed pyrolusite/lignite compound.
（4）Above-mentioned pyrolusite/lignite compound is transferred in tube furnace, in nitrogen atmosphere, with 4OC min-1Speed
It is heated to 450OC, and at this temperature keep 2 it is small when, subsequent cooled to room temperature obtains preconditioning compound；
（5）By above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution press 50:The ratio mixing of 100mL, then mixes this
It closes object to be transferred in autoclave, is heated to 300OWhen C temperature and small holding 1；Room temperature is then cooled to, is filtered, filter residue is used
Neutrality is washed to, the filter residue of gained can use after drying as fuel；Gained filtrate is pyrolusite extracting solution, wherein solvable
The Mn of property2+Content analyzed using conventional atomic absorption spectroscopy, the extraction efficiency for obtaining manganese in pyrolusite is
97%。
Claims (5)
1. a kind of method for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method, it is characterized in that comprising the following steps：
（1）First by pyrolusite solid 80ODried pyrolusite beforehand research is then worn into particle by the air drying of C, then
The pyrolusite particle of this pre-grinding is continued to be ground into pyrolusite powder；
（2）By lignite and 0.5 mol L-1Sulfuric acid solution mixes, 50OIt heats and is sufficiently stirred in C water-baths, filter, washing, institute
Lignite is obtained 80OThe progress beforehand research of dried lignite is then worn into particle by the air drying of C, then by this pre-grinding
Lignite particle continues to be ground into lignite powder；
（3）The pyrolusite powder that above-mentioned grain size is 500 nm or so is mixed with the lignite powder that grain size is 300 nm or so, and
It is fully ground, forms pyrolusite/lignite compound；The pyrolusite powder that the grain size is 500 nm or so and grain size are 300 nm
The mass ratio of the lignite powder of left and right is 1: 1 ~ 5；
（4）By above-mentioned pyrolusite/lignite compound in nitrogen atmosphere, with 4OC min-1Speed be heated to 200OC ~
550OC, and heat preservation a period of time, subsequent cooled to room temperature obtain preconditioning compound at this temperature；
（5）By above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution mixing, the mixture is then transferred to reaction under high pressure
180 are heated in kettleOC ~ 300 OC simultaneously keeps certain time, is subsequently cooled to room temperature, and filtering, gained filtrate is pyrolusite
Then extracting solution extracts violent from pyrolusite extracting solution；The quality of the preconditioning compound and 1 mol L-1Sulfuric acid solution
The ratio between quality volume be 15 ~ 50 g: 100mL.
2. the method according to claim 1 for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method, feature
It is,
Step（1）In, by dried pyrolusite pre-grinding into grain size be the particle of 1 mm or so, then by the soft of this pre-grinding
Manganese ore particle continues to be ground into pyrolusite powder of the grain size for 500 nm or so.
3. the method according to claim 1 for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method, feature
It is,
Step（2）In, be the particle of 1 mm or so by dried lignite pre-grinding, then by the lignite particle of this pre-grinding after
It is continuous to be ground into lignite powder of the grain size for 300 nm or so.
4. the method according to claim 1 for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method, feature
It is,
Step（4）In, the heating temperature is 350OC ~450OC, optimum temperature 400 OC。
5. the method according to claim 1 for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method, feature
It is,
Step（5）In, the heating temperature is 250OC 。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109295305A (en) * | 2018-12-01 | 2019-02-01 | 湖南科技大学 | Lignite recoverying and utilizing method after lignite reductive leaching pyrolusite |
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