CN102367515A - Pressurizing and reductive leaching method of pyrolusite powder - Google Patents
Pressurizing and reductive leaching method of pyrolusite powder Download PDFInfo
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- CN102367515A CN102367515A CN2011103051355A CN201110305135A CN102367515A CN 102367515 A CN102367515 A CN 102367515A CN 2011103051355 A CN2011103051355 A CN 2011103051355A CN 201110305135 A CN201110305135 A CN 201110305135A CN 102367515 A CN102367515 A CN 102367515A
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Abstract
The invention discloses a pressurizing and reductive leaching method of pyrolusite powder. The method comprises the following steps of: a) mixing pyrolusite powder and iron sulfide powder to obtain mixed powder; b) adding a sulphuric acid solution in the mixed powder to pulp and obtain mixed slurry; c) adding the mixed slurry in an autoclave; d) injecting a gas in the autoclave to ensure that the inner pressure of the autoclave reaches a preset pressure value continuously and perform acid leaching under a pressure, then discharging to obtain an acid leaching mixture; and e) performing solid-liquid separation to the acid leaching mixture to obtain a manganese sulfate solution, wherein the pyrolusite powder contains 13-35wt% of manganese. According to the pressurizing and reductive leaching method of pyrolusite powder in the embodiment of the invention, by adopting the pressurizing and leaching method, the manganese in low-grade pyrolusite powder can be leached fast and effectively.
Description
Technical field
The present invention relates to technical field of wet metallurgy, particularly the technical field of wet metallurgy of manganese.
Background technology
The reserves of China's pyrolusite have 5,000 ten thousand tons approximately, and wherein great majority are low-grade lean ore.Current, the poorness of manganese resource is just restricting production and the Sustainable development that China's manganese is product.At some manganese of China is the area that products production is concentrated, and the grade of the manganese carbonate ore that uses is reduced to and has only 13%～15% by containing manganese 18%～20%.And on the other hand, contain the pyrolusite (staple is a Manganse Dioxide) of manganese 20%～25% in a large number, but problem is not used because the too high or contaminate environment of reduction process cost is serious etc.This shows; How economical research, reasonably utilize pyrolusite; Particularly solve the technical problem of its this bottleneck of reducing process; To alleviating current China manganese resource contradiction in short supply, guarantee that manganese is the Sustainable development of product industry, and the west area expanding economy all has crucial strategic importance.
Existing pyrolusite reducing process technology can be divided into roasting method reduction and wet reducing two big classes:
The roasting method reduction is to handle the most current production technique of higher-grade pyrolusite at present.Yet traditional its shortcoming of roasting method reduction is that facility investment flue gas big, that power consumption is high, operational condition is poor, roasting process produces causes severe contamination to environment.
Wet reducing comprises following method:
Two ore deposit single stage method: by certain proportioning, reaction at a certain temperature can make the high price manganese reduction in the pyrolusite generate manganous sulfate with pyrolusite, pyrite and sulfuric acid.Two ore deposits one step lixiviation process current be that to produce manganese be the most current operational path in the product process to the low-grade pyrolusite of China.Yet the shortcoming of two ore deposit single stage method is that reduction ratio and leaching yield are lower, the quantity of slag is big, has influenced the recovery of manganese; Especially on the technology controlling and process of producing the electrolytic metal Mn process, scavenging process is difficult grasps special demands pyrolusite and pyritous mineral resources stable components; Therefore; Though two ore deposit single stage method have obtained using widely in manganous sulfate and the production of regular grade electrolytic manganese dioxide, in the process of producing electrolytic metal Mn, are generally promoted the use of as yet so far.
The sulfurous gas lixiviation process: sulfur dioxide gas feeds in the pyrolusite pulp, can directly carry out reduction reaction and generate manganous sulfate.Yet, though SO
2It is a kind of maturation process that has existed very early that gas directly leaches pyrolusite, but because in this leaching reaction process, has side reaction to produce dithionic acid (MnS
2O
6), influenced the quality of leaching product manganous sulfate, thereby in the production of manganese goods, be not used widely yet so far.
The ferrous sulfate lixiviation process: however iron-holder is higher in the leach liquor of ferrous sulfate leaching pyrolusite, if use current Fe (OH)
3The deironing of neutralization precipitation method will produce a large amount of colloidal precipitation, cause the adsorption losses of filtration difficulty and manganese.
Except that the method for the various leaching pyrolusites of above introduction, also have many lixiviation process to be studied exploitation.Yet the big multipaths of these leaching methods is complicated, or production cost is high, or material corrodibility is strong, and environmental pollution is serious, the unsuitable processing that is applied to low-grade pyrolusite.
Summary of the invention
The present invention is intended to one of solve the problems of the technologies described above at least.For this reason; One object of the present invention is to propose the pressure reduction leaching method of the pyrolusite that a kind of flow process is simple, supplies consumption is few, production cost is low, the treatment time is short, the manganese leaching yield is high; This method can be applicable to low-grade pyrolusite reduction, produces resource utilization, reduces environmental pollution with the manganese ore that improves dilution day by day.
Pressure reduction leaching method according to the pyrolusite powder of the embodiment of the invention may further comprise the steps: a) said pyrolusite powder is mixed with Containing Sulfur iron powder material, obtain mixed powder; B) said mixed powder is sized mixing with sulphuric acid soln, obtain mixed slurry; C) said mixed slurry is added in the autoclave; D) in said autoclave, feed gas and make pressure in the autoclave maintain predetermined force value carrying out pressurized acid leaching, and discharging behind pressurized acid leaching, obtain acidleach and go out mixture; And e) said acidleach is gone out mixture and carry out solid-liquid separation, obtain manganese sulfate solution, wherein, said pyrolusite powder contains the manganese of 13wt%～35wt%.
According to the pressure reduction leaching method of the pyrolusite powder of the embodiment of the invention, because the method that adopts pressurization to leach, the manganese that can will hang down effectively at a high speed in the pyrolusite powder of taste leaches.In addition, it is simple that the pressure reduction leaching method of this pyrolusite powder has technical process, the material low price, and production cost is low, and the treatment time is short, the advantage friendly to physical environment.Simultaneously, adopt the method for the embodiment of the invention, the leaching yield of manganese is high; Realized the stripping of manganese selectivity efficient, simultaneously with Fe, impurity such as Si solidify into slag; Separate impurities such as Mn and Fe is respond well, lays a good foundation for the clean and effective of various valuable elements in the low-grade pyrolusite of final realization reclaims.
In addition, the pressure reduction leaching method of pyrolusite powder according to the above embodiment of the present invention can also have following additional technical characterictic:
Wherein, in order to reduce cost and to improve the leaching yield of manganese in the pyrolusite, in the said step a), said Containing Sulfur iron powder material is a troilite powder, and its granularity is below 100 μ m, and said pyrolusite powder and said troilite powder mix by 1: 0.3～0.5 mass ratio.
Advantageously, in the said step b), the acidity of said sulphuric acid soln is 80g/L～300g/L.
Wherein, in order further to improve the speed of response of pressure reduction, in said step c), the temperature in the said autoclave is controlled at 100 ℃～200 ℃.
Advantageously, in the said step d), said gas is one or more in nitrogen, pressurized air, oxygen enrichment pressurized gas and the industrial pure oxygen.
Advantageously, the force value in the said step d) mesohigh still is 0.1～1.8MPa.
Consider the balance of production cost and leaching yield, in the said step d), the extraction time of said pressurized acid leaching is 30～120min.
According to some embodiments of the present invention, in order to improve the purity of manganese sulfate solution, may further comprise the steps in the said step e): the feed liquid that e-1) will go out behind the still is once filtered, and obtains first-time filtrate; And e-2) in said first-time filtrate, adds cleaner with after removing heavy metal ion wherein, carry out secondary filtration, obtain the high-purity sulphuric acid manganese solution.
Wherein, in order to improve filtration velocity, can adopt vacuum filtration method or filter press technique.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize through practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage obviously with are easily understood becoming the description of embodiment from combining figs, wherein:
Fig. 1 is the process flow sheet according to the pressure reduction leaching method of the pyrolusite powder of the embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of said embodiment is shown in the drawings, and wherein identical from start to finish or similar label is represented identical or similar elements or the element with identical or similar functions.Be exemplary through the embodiment that is described with reference to the drawings below, only be used to explain the present invention, and can not be interpreted as limitation of the present invention.
Pressure reduction leaching method according to the pyrolusite powder of the embodiment of the invention is described with reference to the drawings below.
As shown in the figure, may further comprise the steps according to the pressure reduction leaching method of the pyrolusite powder of the embodiment of the invention.
A) said pyrolusite powder is mixed with Containing Sulfur iron powder material, obtain mixed powder.
Wherein, said pyrolusite powder contains the manganese of 13wt%～35wt%.
Consider that from viewpoints such as cost and speed of response said Containing Sulfur iron powder material can adopt troilite powder, its granularity is below 100 μ m.
Can adjust according to content of effective in each powder about pyrolusite powder and Containing Sulfur iron powder material ratio.Preferably, said pyrolusite powder and said troilite powder mix by 1: 0.3～0.5 mass ratio.
B) said mixed powder is sized mixing with sulphuric acid soln, obtain mixed slurry.
Said sulphuric acid soln does not have particular restriction, but from leaching efficiency, to viewpoints such as the corrosion consideration of autoclave, the sulfuric acid content in the preferred said sulphuric acid soln is 80g/L～300g/L.
C) said mixed slurry is added in the autoclave.
Pressure leaching method of the present invention both can adopt normal temperature to leach also can adopt the high temperature leaching.Consider from improving the leaching efficiency viewpoint, preferably adopt high temperature to leach, the temperature in the said autoclave is controlled at 100 ℃～200 ℃.
D) in said autoclave, feed continuously gas and make pressure in the autoclave maintain predetermined force value carrying out pressurized acid leaching, and discharging behind pressurized acid leaching, obtain acidleach and go out mixture.
Do not have special limitation about said gas, for example can be in nitrogen, pressurized air, oxygen enrichment pressurized air and the industrial pure oxygen one or more.
Time about pressurized acid leaching can and combine leaching efficiency, cost suitably to regulate according to conditions such as raw material, pressure, temperature, and for example, the extraction time of said pressurized acid leaching can be controlled at 30～120min.
About force value, volume that can the association reaction still, the compressive property of reaction kettle wait and set, and preferably, make the pressure in the autoclave maintain 0.1～1.8MPa.
Contingent principal reaction formula is in low-grade pyrolusite and the sulfurous iron ore pressure reduction leaching process:
FeS
2+MnO
2+4H
+＝Fe
2++Mn
2++2H
2O+2S
2- (1)
2FeS
2+15MnO
2+22H
+＝Fe
2O
3+15Mn
2++11H
2O+4SO
4 2- (2)
FeS
2+7MnO
2+14H
+＝Fe
2++7Mn
2++6H
2O+2HSO
4 - (3)
2FeS
2+15MnO
2+14H
2SO
4＝15MnSO
4+Fe
2(SO
4)
3+14H
2O (4)
2FeS
2+3MnO
2+6H
2SO
4＝3MnSO
4+Fe
2(SO
4)
3+6H
2O+4S (5)
FeS
2+MnO
2+2H
2SO
4＝MnSO
4+FeSO
4+2H
2O+2S (6)
2FeS
2+9MnO
2+10H
2SO
4＝9MnSO
4+Fe
2(SO
4)
3+2S+10H
2O (7)
2FeS
2+15MnO
2+7H
2SO
4＝9MnSO
4+2Fe(OH)
3+2S+14H
2O (8)
Can know by above-mentioned reaction formula; After the process pressurized acid leaching went out, the tetravalence manganese in the pyrolusite was reduced to the bivalent manganese of solubility, that is to say that the form with manganous sulfate exists in acid leaching liquor; And impurity such as Fe, S are cured into slag, thereby can realize the high efficiency separation of impurity such as Mn and Fe.
E) said acidleach is gone out mixture and carry out solid-liquid separation, obtain manganese sulfate solution.
The concrete solid-liquid separating method that is adopted comprises filtration, sedimentation etc.Wherein, from considerations such as raising filtration velocity, can adopt vacuum filtration or press filtration.
In examples more of the present invention, in order to improve the purity of gained manganese sulfate solution, this step specifically can may further comprise the steps: the feed liquid that e-1) will go out behind the still is once filtered, and obtains first-time filtrate; And e-2) in said first-time filtrate, adds cleaner with after removing heavy metal ion wherein, carry out secondary filtration, obtain the high-purity sulphuric acid manganese solution.
Below through the pressure reduction leaching method of specific embodiment explanation according to pyrolusite powder of the present invention.
Embodiment one: contain manganese grade 21.14wt% in the low-grade pyrolusite.
The low-grade pyrolusite powder that will contain manganese 21.14% mixes with the levigated troilite powder, uses acid concentration to size mixing as the sulphuric acid soln of 140g/L mixed mineral powder; Slip after sizing mixing joins in the acidproof autoclave of titanium matter of 2L, feeds pressurized air continuously, keeps still internal pressure 0.5MPa, 120 ℃ of temperature, the leaching of pressurizeing, extraction time 60min.Carry out solid-liquid separation after going out still, obtain manganese sulfate solution.
Embodiment two: low-grade pyrolusite contains manganese grade 28.38%.。
The low-grade pyrolusite powder that will contain manganese 28.38% mixes with the levigated troilite powder, uses acid concentration to size mixing as the sulphuric acid soln of 120g/L mixed mineral powder; Slip after sizing mixing joins in the acidproof autoclave of titanium matter of 2L, feeds nitrogen continuously, keeps still internal pressure 0.8Mpa, 100 ℃ of temperature, the leaching of pressurizeing, extraction time 120min.Carry out solid-liquid separation after going out still, obtain manganese sulfate solution.
Embodiment three: low-grade pyrolusite contains manganese grade 26.53%.
The low-grade pyrolusite powder that will contain manganese 26.53% mixes with the levigated troilite powder, uses acid concentration to size mixing as the sulphuric acid soln of 80g/L mixed mineral powder; Slip after sizing mixing joins in the acidproof autoclave of titanium matter of 2L, feeds pressurized air continuously, keeps still internal pressure 1.2Mpa, 150 ℃ of temperature, the leaching of pressurizeing, extraction time 90min.Carry out solid-liquid separation after going out still, obtain manganese sulfate solution.
Embodiment four: low-grade pyrolusite contains manganese grade 17.64%.
The low-grade pyrolusite powder that will contain manganese 17.64% mixes with the levigated troilite powder, uses acid concentration to size mixing as the sulphuric acid soln of 120g/L mixed mineral powder; Slip after sizing mixing joins in the acidproof autoclave of titanium matter of 2L, feeds pressurized air continuously, keeps still internal pressure 1.4Mpa, 140 ℃ of temperature, the leaching of pressurizeing, extraction time 30min.Carry out solid-liquid separation after going out still, obtain manganese sulfate solution.
Embodiment five: low-grade pyrolusite contains manganese grade 35%.
The low-grade pyrolusite powder that will contain manganese 35% mixes with the levigated troilite powder, uses acid concentration to size mixing as the sulphuric acid soln of 120g/L mixed mineral powder; Slip after sizing mixing joins in the acidproof autoclave of titanium matter of 2L, feeds compressed nitrogen continuously, keeps still internal pressure 0.8Mpa, 120 ℃ of temperature, the leaching of pressurizeing, extraction time 60min.Carry out solid-liquid separation after going out still, obtain manganese sulfate solution.
Embodiment six: low-grade pyrolusite contains manganese grade 15%.
This smoke dust is mixed with the levigated troilite powder, use acid concentration to size mixing mixed mineral powder as the sulphuric acid soln of 140g/L; Slip after sizing mixing joins in the acidproof autoclave of titanium matter of 2L, feeds the compression oxygen-rich air continuously, keeps still internal pressure 1.8Mpa, 150 ℃ of temperature, the leaching of pressurizeing, extraction time 120min.Carry out solid-liquid separation after going out still, obtain manganese sulfate solution.
Estimate for the pressure reduction leaching method effect to pyrolusite powder of the present invention, resulting manganese sulfate solution of above-mentioned each embodiment and leached mud have been carried out following analysis, analytical results is as shown in table 1.
1) manganese leaching yield
Calculate the manganese leaching yield according to the following equation.
Manganese leaching yield=(1-C
1M
1/ M) * 100%
Wherein: M---manganese element total mass (unit: g) in the raw material
C
1---the quality percentage composition (unit: wt%) of manganese element in the filter residue
M
1---the quality (unit: g) of filter residue
2) slag rate
Calculate the slag rate according to the following equation.
Slag rate=(M
4/ M
3) * 100%
Wherein: M
3---raw material ore deposit total mass (unit: g)
M
4---the quality (unit: g) of filter residue
Table 1
Can find out by table 1; With the manganese grade at the low-grade pyrolusite of 15wt%～35wt% with after sulfurous iron ore mixes, size mixing with the sulfuric acid concentration of acid concentration 80～300g/L, put into autoclave and carry out pressurized acid leaching; The leaching yield of manganese all can realize more than 95%; The leaching yield of manganese is high, has realized the selectivity efficient stripping of Mn, lays a good foundation for the clean and effective of various valuable elements in the low-grade pyrolusite of final realization reclaims.In addition, as raw material, raw material sources are wide, and are cheap with low-grade pyrolusite and sulfurous iron ore, and production cost is low, and operating process is simple, and extraction time is short.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means the concrete characteristic, structure, material or the characteristics that combine this embodiment or example to describe and is contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete characteristic, structure, material or the characteristics of description can combine with suitable manner in any one or more embodiment or example.
Although illustrated and described embodiments of the invention; Those having ordinary skill in the art will appreciate that: under the situation that does not break away from principle of the present invention and aim, can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited claim and equivalent thereof.
Claims (9)
1. the pressure reduction leaching method of a pyrolusite powder is characterized in that, may further comprise the steps:
A) said pyrolusite powder is mixed with Containing Sulfur iron powder material, obtain mixed powder;
B) said mixed powder is sized mixing with sulphuric acid soln, obtain mixed slurry;
C) said mixed slurry is added in the autoclave;
D) in said autoclave, feed gas and make pressure in the autoclave maintain predetermined force value carrying out pressurized acid leaching, and discharging behind pressurized acid leaching, obtain acidleach and go out mixture; With
E) said acidleach is gone out mixture and carries out solid-liquid separation, obtain manganese sulfate solution,
Wherein, said pyrolusite powder contains the manganese of 13wt%～35wt%.
2. the pressure reduction leaching method of pyrolusite powder according to claim 1; It is characterized in that in the said step a), said Containing Sulfur iron powder material is a troilite powder; Its granularity is below 100 μ m, and said pyrolusite powder and said troilite powder mix by 1: 0.3～0.5 mass ratio.
3. the pressure reduction leaching method of pyrolusite powder according to claim 1 is characterized in that, in the said step b), the acidity of said sulphuric acid soln is 80g/L～300g/L.
4. the pressure reduction leaching method of pyrolusite powder according to claim 1 is characterized in that, in said step c), the temperature in the said autoclave is controlled at 100 ℃～200 ℃.
5. the pressure reduction leaching method of pyrolusite powder according to claim 1 is characterized in that, in the said step d), said gas is one or more in nitrogen, pressurized air, oxygen enrichment pressurized gas and the industrial pure oxygen.
6. the pressure reduction leaching method of pyrolusite powder according to claim 1 is characterized in that, the force value in the said step d) mesohigh still is 0.1～1.8MPa.
7. according to the pressure reduction leaching method of each described pyrolusite powder among the claim 1-6, it is characterized in that in the said step d), the extraction time of said pressurized acid leaching is 30～120min.
8. according to the pressure reduction leaching method of each described pyrolusite powder among the claim 1-7, it is characterized in that, may further comprise the steps in the said step e):
The feed liquid that e-1) will go out behind the still is once filtered, and obtains first-time filtrate; With
E-2) in said first-time filtrate, add cleaner with after removing heavy metal ion wherein, carry out secondary filtration, obtain the high-purity sulphuric acid manganese solution.
9. the pressure reduction leaching method of pyrolusite powder according to claim 8 is characterized in that, vacuum filtration method or filter press technique are adopted in said filtration.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103051355A CN102367515A (en) | 2011-10-10 | 2011-10-10 | Pressurizing and reductive leaching method of pyrolusite powder |
| CN2012101184287A CN102618728A (en) | 2011-10-10 | 2012-04-20 | Method for producing manganese sulfate by leaching manganese alloy slag under normal pressure |
| CN2012101183566A CN102605186A (en) | 2011-10-10 | 2012-04-20 | Method for producing manganese sulfate from manganese-rich slag through atmospheric pressure leaching |
| CN2012101183886A CN102605187A (en) | 2011-10-10 | 2012-04-20 | Method for producing manganese sulfate by manganese-rich slag through pressure leaching |
| CN201210118398XA CN102605188A (en) | 2011-10-10 | 2012-04-20 | Method for producing manganese sulfate by manganese alloy slag through pressure leaching |
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| CN2011103051355A CN102367515A (en) | 2011-10-10 | 2011-10-10 | Pressurizing and reductive leaching method of pyrolusite powder |
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- 2011-10-10 CN CN2011103051355A patent/CN102367515A/en not_active Withdrawn
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| CN103757228B (en) * | 2013-12-29 | 2016-01-20 | 四川师范大学 | The leaching method of pyrolusite |
| CN103757219B (en) * | 2013-12-29 | 2016-02-24 | 四川师范大学 | The leaching method of pyrolusite |
| CN103757233B (en) * | 2013-12-29 | 2016-02-24 | 四川师范大学 | The leaching method of pyrolusite |
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| CN112777642B (en) * | 2021-01-26 | 2023-03-14 | 广西埃索凯新材料科技有限公司 | Method for preparing high-purity manganese sulfate by reducing and leaching pyrolusite by using rotary kiln slag |
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