CN108085486B - A method of manganese being extracted from low-grade pyrolusite with grinding-pressurization combination method - Google Patents
A method of manganese being extracted from low-grade pyrolusite with grinding-pressurization combination method Download PDFInfo
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- CN108085486B CN108085486B CN201810029181.9A CN201810029181A CN108085486B CN 108085486 B CN108085486 B CN 108085486B CN 201810029181 A CN201810029181 A CN 201810029181A CN 108085486 B CN108085486 B CN 108085486B
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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 methods that manganese is extracted from low-grade pyrolusite with grinding-pressurization combination method, comprising steps of dry pyrolusite is formed pyrolusite powder by (1) after grinding step by step；(2) by lignite with 0.5 mol L‑1Re-dry after sulfuric acid solution, forms lignite powder after grinding step by step；(3) above-mentioned pyrolusite powder is mixed with lignite powder, and be fully ground, form 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, is obtained 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 be used as fuel use after drying.Cost of material of the 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, soaks from low-grade pyrolusite
The technique of manganese out, belongs to field of hydrometallurgy.
Background technique
Manganese product in people's daily life with have highly important effect in industrial and agricultural production.Currently, manganese product
It is mainly used in alloy field, 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 foreign countries, how to develop
It is an important project that manganese resource using China, which is national economy service,.
Low-grade pyrolusite (Mn% < 40%) is relatively more in the west and south in China, but how to extract manganese therein, especially
This key technical problem of reducing process how is solved, is still the important link of pyrolusite development and 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.
Currently, 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- in reduction roasting temperature
At 900 DEG C, manganese dioxide is finally reduced to divalent manganese oxide in pyrolusite, to extract manganese in an acidic solution.Reduction
Reducing agent generallys use the reducing substances such as coal dust, carbon monoxide, hydrogen, methane in the process.The method will be used in reduction process
The equipment such as reverberatory furnace, reduction furnace, rotary kiln, and cooling water is also sprayed after high-temperature roasting is quickly cooled down rotary kiln, otherwise, generates
Manganese oxide can be oxidized to manganese sesquioxide managnic oxide in air.The manganese oxide of generation is basic anhydride, it is easy to dilute sulfuric acid
React in addition, the major defect of the method is to consume a large amount 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 mature, 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 mine 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 mine one-step method can be anti-
A step in slot is answered to complete, process flow is simple, and pyrite is resourceful, can meet the needs of pyrolusite reduction, to a certain extent
Improve the environment of worker 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 Xie Meng and manganese dioxide technique.In addition, the method can also generate a large amount of waste residue, subsequent processing is more troublesome.
(4) organic matter reduction method: using organic matters conducts such as glucose, sucrose, lactose, crop products or byproducts
Reducing agent can react with the manganese dioxide in pyrolusite in acidic 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 thoroughly to generate a small amount of small molecule and be dissolved in leachate, it is not easy purification completely, especially in electrolytic industry, on a small quantity
Organic matter, which this may result in electrolysis, cannot proceed normally.
(5) hydrogen peroxide reduction method: when making reducing agent with hydrogen peroxide, will consume more hydrogen peroxide, and the price of the latter is higher,
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
Out.But for leach 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,
It is directly added into sponge iron, 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 methods is inherently essentially identical, but in their subsequent processes, a large amount of iron hydroxide is separated
It removes, that there are processes 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
Close object therefore pyrolusite is restored using it as reducing agent, thus extract manganese be it is feasible, from the comprehensive utilization of lignite
With important practical significance.
The present invention is using lignite as reducing agent, in an acidic solution, will be in pyrolusite by improving reaction temperature and pressure
Value Mn be reduced to soluble bivalent manganese, to realize that low cost, high efficiency extract the process of manganese.Since this is solid-solid-
Reaction between liquid, so lignite and pyrolusite particle are fully ground powdering particle respectively first by the present invention；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 adequately, to be very beneficial for their subsequent reactions.Then by them in sulfuric acid solution
Middle carry out ultrasonic disperse；It is finally sufficiently reacted in hydrothermal reaction kettle again, manganese reduction, the leaching in pyrolusite is come out, filtered
Slag can be used as fuel use after drying.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.
Summary of the invention
The object of the present invention is to provide a kind of methods that manganese is extracted from low-grade pyrolusite with grinding-pressurization combination method.
Embodiment of the present invention are as follows: a method of manganese is extracted from low-grade pyrolusite with grinding-pressurization combination method,
The following steps are included:
(1) first by pyrolusite solid 80OThe air drying of C then wears into the pyrolusite beforehand research after drying
Grain, then continue the pyrolusite particle of this pre-grinding to be ground into pyrolusite powder；
(2) by lignite and 0.5 mol L-1Sulfuric acid solution mixing, 50OIt heats and is sufficiently stirred in C water-bath, filter, water
It washes, gained lignite is 80OLignite after drying is then carried out beforehand research and wears into particle by the air drying of C, then by this beforehand research
The lignite particle of mill continues to be ground into lignite powder；
(3) pyrolusite powder that above-mentioned partial size is 500 nm or so is mixed with lignite powder that partial size is 300 nm or so
It closes, and is fully ground, form pyrolusite/lignite compound；The pyrolusite powder that the partial size is 500 nm or so is with partial size
The mass ratio of the lignite powder of 300 nm or so 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 high pressure
180 are heated in reaction kettleOC ~ 300 OC simultaneously keeps certain time, then cools to room temperature, filtering, and gained filtrate is as soft
Then manganese ore extracting solution extracts violent from pyrolusite extracting solution；The quality of the preconditioning compound and 1 mol L-1Sulfuric acid
The ratio between quality volume of solution is 15 ~ 50 g: 100mL.
Preferably, in step (1), the particle for being 1 mm or so at partial size by the pyrolusite pre-grinding after drying, then will
The pyrolusite particle of this pre-grinding continues to be ground into the pyrolusite powder that partial size is 500 nm or so.
Preferably, in step (2), the particle for being 1 mm or so by the lignite pre-grinding after drying, then by this beforehand research
The lignite particle of mill continues to be ground into the lignite powder that partial size is 300 nm or so.
Preferably, the heating temperature is 350 in step (4)OC ~450OC, optimum temperature 400 OC。
Preferably, the heating temperature is 250 in step (5)OC 。
The present invention forms the very big little particle of surface area, to guarantee soft manganese by the way that pyrolusite and lignite to be fully ground
Mine has sufficient contact area when reacting with both solid matters of lignite；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 the value Mn partial reduction in pyrolusite be enable to be low price manganese；Finally again
It is reacted by high temperature, high-pressure leaching, leaches the value Mn in pyrolusite completely and come out, and resulting filter residue is not predominantly anti-
It answers or the lesser lignite of the extent of reaction, can be used as fuel use after drying.Cost of material of the 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 80OIt is 24 hours dry in the air drying cabinet of C；Then by the soft manganese after drying
Mine, which is placed in general milling machine, carries out pre-grinding, is ground into the particle that partial size is 1 mm or so；Again by this pre-grinding
Pyrolusite particle is transferred in high speed ball mill, it is continued to be ground into the pyrolusite powder that partial size is 500 nm or so.
(2) by lignite and 0.5 mol L-1Sulfuric acid solution mixing, 50OIt heats and stirs 3 hours in C water-bath；Subsequent mistake
Filter, is washed with water twice, gained lignite is 80OIt is 24 hours dry in the air drying cabinet of C；Then the lignite after drying is placed in general
Pre-grinding is carried out in logical ball mill, is ground into the particle that partial size is 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 the lignite powder that partial size is 300 nm or so.
(3) it is the lignite powder of 300 nm or so by 1 by pyrolusite powder and partial size that above-mentioned partial size is 500 nm or so:
1 mass ratio, which is placed in high speed ball mill, to be mixed, and is fully ground 0.5 ~ 1.5 hour, and pyrolusite/lignite compound is formed.
(4) above-mentioned pyrolusite/lignite compound is transferred in tube furnace, in nitrogen atmosphere, with 4OC min-1Speed
It is heated to 200OC, and kept for 2 hours at this temperature, subsequent cooled to room temperature obtains preconditioning compound；
(5) by above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution in 15:100mL ratio mix, then will
The mixture is transferred in autoclave, is heated to 180OC temperature is simultaneously kept for 4 hours；It is then cooled to room temperature, is filtered, filter
Slag is washed with water to neutrality, and resulting filter residue can be used as fuel use after drying；Gained filtrate is pyrolusite extracting solution, wherein
Soluble Mn2+Content analyzed using conventional atomic absorption spectroscopy, obtain the extraction effect of manganese in pyrolusite
Rate is 93%.
Embodiment 2:
(1) first by pyrolusite solid 80OIt is 24 hours dry in the air drying cabinet of C；Then by the soft manganese after drying
Mine, which is placed in general milling machine, carries out pre-grinding, is ground into the particle that partial size is 1 mm or so；Again by this pre-grinding
Pyrolusite particle is transferred in high speed ball mill, it is continued to be ground into the pyrolusite powder that partial size is 500 nm or so.
(2) by lignite and 0.5 mol L-1Sulfuric acid solution mixing, 50OIt heats and stirs 3 hours in C water-bath；Subsequent mistake
Filter, is washed with water twice, gained lignite is 80OIt is 24 hours dry in the air drying cabinet of C；Then the lignite after drying is placed in general
Pre-grinding is carried out in logical ball mill, is ground into the particle that partial size is 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 the lignite powder that partial size is 300 nm or so.
(3) it is the lignite powder of 300 nm or so by 1 by pyrolusite powder and partial size that above-mentioned partial size is 500 nm or so:
2 mass ratio, which is placed in high speed ball mill, to be mixed, and is fully ground 1 hour, and pyrolusite/lignite compound is formed.
(4) above-mentioned pyrolusite/lignite compound is transferred in tube furnace, in nitrogen atmosphere, with 4OC min-1Speed
It is heated to 300OC, and kept for 2 hours at this temperature, subsequent cooled to room temperature obtains preconditioning compound；
(5) by above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution in 30:100mL ratio mix, then will
The mixture is transferred in autoclave, is heated to 240OC temperature is simultaneously kept for 2 hours；It is then cooled to room temperature, is filtered, filter
Slag is washed with water to neutrality, and resulting filter residue can be used as fuel use after drying；Gained filtrate is pyrolusite extracting solution, wherein
Soluble Mn2+Content analyzed using conventional atomic absorption spectroscopy, obtain the extraction effect of manganese in pyrolusite
Rate is 96%.
Embodiment 3:
(1) first by pyrolusite solid 80OIt is 24 hours dry in the air drying cabinet of C；Then by the soft manganese after drying
Mine, which is placed in general milling machine, carries out pre-grinding, is ground into the particle that partial size is 1 mm or so；Again by this pre-grinding
Pyrolusite particle is transferred in high speed ball mill, it is continued to be ground into the pyrolusite powder that partial size is 500 nm or so.
(2) by lignite and 0.5 mol L-1Sulfuric acid solution mixing, 50OIt heats and stirs 3 hours in C water-bath；Subsequent mistake
Filter, is washed with water twice, gained lignite is 80OIt is 24 hours dry in the air drying cabinet of C；Then the lignite after drying is placed in general
Pre-grinding is carried out in logical ball mill, is ground into the particle that partial size is 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 the lignite powder that partial size is 300 nm or so.
(3) it is the lignite powder of 300 nm or so by 1 by pyrolusite powder and partial size that above-mentioned partial size is 500 nm or so:
5 mass ratio, which is placed in high speed ball mill, to be mixed, and is fully ground 1.5 hours, and pyrolusite/lignite compound is formed.
(4) above-mentioned pyrolusite/lignite compound is transferred in tube furnace, in nitrogen atmosphere, with 4OC min-1Speed
It is heated to 450OC, and kept for 2 hours at this temperature, subsequent cooled to room temperature obtains preconditioning compound；
(5) by above-mentioned preconditioning compound and 1 mol L-1Sulfuric acid solution in 50:100mL ratio mix, then will
The mixture is transferred in autoclave, is heated to 300OC temperature is simultaneously kept for 1 hour；It is then cooled to room temperature, is filtered, filter
Slag is washed with water to neutrality, and resulting filter residue can be used as fuel use after drying；Gained filtrate is pyrolusite extracting solution, wherein
Soluble Mn2+Content analyzed using conventional atomic absorption spectroscopy, obtain the extraction effect of manganese in pyrolusite
Rate is 97%.
Claims (4)
1. a kind of method that manganese is extracted from low-grade pyrolusite with grinding-pressurization combination method, it is characterized in that the following steps are included:
(1) the pyrolusite beforehand research after drying is then worn into particle by the air drying first by pyrolusite solid at 80 DEG C, then
The pyrolusite particle of this pre-grinding is continued to be ground into partial size to be 500 nm pyrolusite powder；
(2) by lignite and 0.5 mol L-1Sulfuric acid solution mixing, heats and is sufficiently stirred in 50 DEG C of water-baths, filters, washing,
Lignite after drying is then carried out beforehand research and wears into particle by air drying of the gained lignite at 80 DEG C, then by this pre-grinding
Lignite particle to continue to be ground into partial size be 300 nm lignite powders；
(3) the pyrolusite powder that above-mentioned partial size is 500 nm is mixed with the lignite powder that partial size is 300 nm, and is fully ground,
Form pyrolusite/lignite compound；The lignite powder that the pyrolusite powder and partial size that the partial size is 500 nm are 300 nm
Mass ratio is 1: 1 ~ 5；
(4) by above-mentioned pyrolusite/lignite compound in nitrogen atmosphere, with 4 DEG C of min-1Speed be heated to 200 DEG C ~ 550
DEG C, 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 molL-1Sulfuric acid solution mixing, the mixture is then transferred to reaction under high pressure
It is heated to 180 DEG C ~ 300 DEG C in kettle and keeps certain time, then cools to room temperature, filters, gained filtrate is that pyrolusite mentions
Liquid is taken, then extracts manganese from pyrolusite extracting solution；The quality of the preconditioning compound and 1 molL-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 that heating temperature described in step (4) is 350 DEG C ~ 450 DEG C.
3. the method according to claim 2 for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method, feature
It is that the heating temperature is 400 DEG C.
4. the method according to claim 1 for extracting manganese from low-grade pyrolusite with grinding-pressurization combination method, feature
It is that heating temperature described in step (5) is 250 DEG C.
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