CN102618728A - Method for producing manganese sulfate by leaching manganese alloy slag under normal pressure - Google Patents
Method for producing manganese sulfate by leaching manganese alloy slag under normal pressure Download PDFInfo
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- CN102618728A CN102618728A CN2012101184287A CN201210118428A CN102618728A CN 102618728 A CN102618728 A CN 102618728A CN 2012101184287 A CN2012101184287 A CN 2012101184287A CN 201210118428 A CN201210118428 A CN 201210118428A CN 102618728 A CN102618728 A CN 102618728A
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Abstract
The invention discloses a method for producing manganese sulfate by leaching manganese alloy slag under normal pressure. The method comprises the following steps of: a) mixing the manganese iron alloy slag and a sulfuric acid solution to obtain mixed slurry; b) adding the mixed slurry into a reaction container; c) controlling the pH value of the solution in the reaction process, and discharging after normal pressure acid leaching to obtain an acid leached mixture; and d) performing solid-liquid separation on the acid leached mixture to obtain a manganese sulfate solution. According to the method for producing the manganese sulfate by leaching the manganese alloy slag under the normal pressure, the leaching rate of manganese is high, and selective efficient dissolution of the manganese is realized. Moreover, the method for producing the manganese sulfate by leaching the manganese alloy slag under the normal pressure has the advantages of simple process flow, cheap materials, low production cost, short treatment time and natural environment friendliness.
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 manganese alloy slag derives from The ferroalloy industry usually, and its chemical ingredients mainly contains SiO
2, Al
2O
3, CaO, MgO, FeO, MnO, MnS etc.The most of method of shrend that adopts of manganese and manganese alloy slag is washed into grain slag at present, and as the grog of cement, at present, blast furnace ferromanganese slag, manganese-silicon slag, high carbon ferromanganese slag all adopt the shrend method to handle, and the shrend method comprises: stokehold water quenching and tank switching water quenching.The present comprehensive utilization method of manganese metallurgical slag has: the manganese metallurgical slag recycles directly that (for example: electric furnace high carbon ferromanganese slag can be used to smelt manganese-silicon; Utilize the manganese-silicon slag can smelt complex ferroalloy; Utilize the manganese metal slag can produce complex ferroalloy); The manganese alloy slag is done cast stone; The manganese alloy slag is done slag wool (lagging material); The manganese alloy slag is done material of construction; The manganese alloy slag is done farmland fertilizer.But existing manganese alloy slag utilizes technology to have waste and environmental pollution problems.
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 manganese alloy slag normal pressure 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 and leaches the method for producing manganous sulfate; This method can solve manganeseirom slag in the past and utilize technology to take the big area place and to the pollution problem of environment; Make manganese resource in the manganeseirom slag obtain the utilization of economical rationality, the manganese ore that improves dilution day by day produces resource utilization.
Manganese alloy slag normal pressure according to the embodiment of the invention leaches the method for producing manganous sulfate, may further comprise the steps: a) said manganese alloy slag is sized mixing with sulphuric acid soln, obtain mixed slurry; B) said mixed slurry is added in the reaction vessel; C) the pH value of control solution in reaction process, and discharging after the normal pressure acidleach obtains acidleach and goes out mixture; And d) said acidleach is gone out mixture and carry out solid-liquid separation, obtain manganese sulfate solution.
Manganese alloy slag normal pressure according to the embodiment of the invention leaches the method for producing manganous sulfate, and the leaching yield of manganese is high, has realized the stripping of manganese selectivity efficient.In addition, it is simple that the method that manganous sulfate is produced in this manganese alloy slag normal pressure leaching has technical process, the material low price, and production cost is low, and the treatment time is short, the advantage friendly to physical environment.
In addition, the method for manganese alloy slag normal pressure leaching production manganous sulfate according to the above embodiment of the present invention can also have following additional technical characterictic:
Wherein, improve the leaching yield of manganese in the manganese alloy slag and accelerate leaching velocity, in the said step a), said manganeseirom slag refers to (Water Quenching Slag that comprises them) such as carbon-manganese alloy slag and manganese-silicon slags, and granularity is controlled at more than 100 orders.Advantageously, in the said step b), the initial acidity of said sulphuric acid soln is 1g/L～100g/L, and the liquid-solid ratio in the said mixed slurry is 3: 1～16: 1.
Wherein, in order further to improve the speed of response that normal pressure leaches, in said step c), the temperature in the said reaction vessel is controlled at 50 ℃～98 ℃.
Consider the balance of production cost and leaching yield, in the said step d), the extraction time that said normal pressure leaches is 60～120min.
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 d): d-1) add manganese alloy slag and quicklime in the slip after going out reaction vessel, making its pH value is in 6.5～7 scopes so that neutralization acid wherein; And d-2) slip after neutralizing treatment once filters, washs, and obtains manganous sulfate filtrating and leached mud.
Wherein, can be with the raw material of said leached mud as the preparation molecular sieve.
In addition, in order to improve the quality of manganous sulfate filtrating, step d) further comprises: d-3) in said manganous sulfate filtrating, add scavenging agent with after removing heavy metal ion wherein, carry out secondary filtration, washing, obtain the high-purity sulphuric acid manganese solution.Said scavenging agent can be Sodium Dimethyldithiocarbamate ((CH
3)
2NCS
2Na), be called for short SDD).
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 that leaches the method for producing manganous sulfate according to the manganese alloy slag normal pressure 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.
The manganese alloy slag normal pressure that is described with reference to the drawings below according to the embodiment of the invention leaches the method for producing manganous sulfate.
As shown in the figure, the method for producing manganous sulfate according to the manganese alloy slag normal pressure leaching of the embodiment of the invention may further comprise the steps.
A) said manganese alloy slag is sized mixing with sulphuric acid soln, obtain mixed slurry.
Because the leaching raw material of present method is the manganese alloy slag, considers that the manganese alloy slag is resulting via method of reducing, manganese nearly all exists with the form of bivalent manganese, needn't consider the reduction problem so segmented acid-adding normal pressure acidleach manganese alloy slag prepares in the process of manganous sulfate.
The leaching agent that is adopted is a sulfuric acid, and the purpose of leaching is to make the manganese in the manganese alloy slag obtain higher leaching yield as far as possible, and from slag, being dissolved out becomes water miscible manganous sulfate.
Consider that from viewpoints such as cost and speed of response the granularity of said manganese alloy slag is controlled at more than 100 orders.
Said sulphuric acid soln does not have particular restriction, but from leaching efficiency, to viewpoints such as the corrosion consideration of reaction vessel, the initial acidity of preferred said sulphuric acid soln is 1g/L～100g/L.In addition, can set according to the content of effective constituent separately about the ratio of manganese alloy slag and sulphuric acid soln.Liquid-solid ratio in the said mixed slurry is 3: 1～16: 1.
B) said mixed slurry is added in the reaction vessel.
Consider from improving the leaching efficiency viewpoint, the temperature in the said reaction vessel is controlled at 50 ℃～98 ℃.
C) the pH value of control solution in leaching process, and discharging after the normal pressure acidleach obtains acidleach and goes out mixture.
Time about the normal pressure acidleach can and combine leaching efficiency, cost suitably to regulate according to conditions such as raw material, temperature, and for example, the extraction time of said normal pressure acidleach can be controlled at 60～120min.
In the acidleach process, reactions mainly takes place:
MnO+H
2SO
4→MnSO
4+H
2O (1)
Al
2O
3(amorphous)+H
2SO
4→ Al
2(SO
4)
3+ H+H
2O (2)
MnSiO
3+H
2SO
4→MnSO
4+H
2SiO
3+H2O (3)
Mn(AlO
2)
2+H
2SO
4→MnSO
4+H
3AlO
3+H2O (4)
Fe+H
2SO
4→FeSO
4+H
2↑ (5)
FeO+H
2SO
4→FeSO
4+H
2O (6)
FeS+H
2SO
4→FeSO
4+H
2S↑ (7)
CaO+H
2SO
4→CaSO
4+H
2O (8)
Can know that by above-mentioned reaction formula after acidleach went out through normal pressure, the manganese in the manganese alloy slag was converted into water miscible manganous sulfate and is dissolved in the leach liquor, and impurity such as Fe, Si, Al are cured into slag, thereby can realize the high efficiency separation of Mn and impurity such as Fe, Si.
D) 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:
D-1) add manganese alloy slag and quicklime in the slip after going out reaction vessel to make its pH value be in 6.5～7 scopes so that neutralize wherein acid.
In the acidleach process, in order to improve leaching efficiency, total acid content is far above the acid of chemical theory amount; Therefore also remaining in the slip after the acidleach have a certain amount of acid; For this reason, in embodiment once of the present invention, through adding manganese alloy slag and the quicklime spent acid wherein that neutralizes.Mainly utilize the wherein most acid that neutralizes of manganese alloy slag, and utilize in the quicklime and remaining small amount of acid.In the time of in pH value of slurry is 6.5～7 scopes, can think that spent acid is wherein neutralized by the overwhelming majority.
Can wait aptly according to the manganese content in employed vitriolic acidity, liquid-solid ratio and the manganese alloy slag in the acidleach process about the concrete amount of manganese alloy slag and quicklime and set.
D-2) slip after neutralizing treatment once filters, washs, and obtains manganous sulfate filtrating and leached mud.
Wherein, because leached mud contains SiO
2And Al
2O
3More, can be with the raw material of said leached mud as the preparation molecular sieve.
In addition, in order further to improve the quality of manganous sulfate filtrating, can further include following steps:
D-3) in said manganous sulfate filtrating, add scavenging agent, carry out secondary filtration, washing, obtain the high-purity sulphuric acid manganese solution with after removing heavy metal ion wherein.
Wherein, said scavenging agent can adopt Sodium Dimethyldithiocarbamate (SDD).
Leach the method for producing manganous sulfate according to manganese alloy slag normal pressure of the present invention through the specific embodiment explanation below.
Embodiment one:
Carbon-manganese alloy slag ore deposit is finely ground to the breeze of mean particle size more than 100 orders, gets 100g; Use and initially contain acid concentration and size mixing liquid-solid ratio 15: 1 as the sulphuric acid soln of 90g/L; Slip after sizing mixing adds in the reaction vessel, and controlled temperature is at 98 ℃; Reaction times is discharging behind 120min; Add a small amount of manganese alloy slag in the slip after going out reaction vessel, neutralize most spent acid, add again among the proper C aO and remaining a small amount of spent acid, until the pH value between 6.5 to 7; Filter washing then; The leached mud that obtains behind the filtration washing is as the raw material of sub products such as preparation molecular sieve; After first-time filtrate added scavenging agent SDD degree of depth removing heavy metals ion, carry out secondary filtration, washing; At last, the manganese sulfate solution that obtains is sent to the potroom preparing electrolyte.
Embodiment two:
Carbon-manganese alloy slag ore deposit is finely ground to the breeze of mean particle size more than 100 orders, gets 100g; Use and initially contain acid concentration and size mixing liquid-solid ratio 8: 1 as the sulphuric acid soln of 50g/L; Slip after sizing mixing adds in the reaction vessel, and controlled temperature is at 50 ℃; The pH value of control solution is in certain scope in leaching process, and the reaction times is discharging behind 100min; Add a small amount of manganese alloy slag in the slip after going out reaction vessel, neutralize most spent acid, add among the proper C aO again and remaining a small amount of spent acid, regulate the pH value between 6.5 to 7; Filter washing then; The leached mud that obtains behind the filtration washing is as the raw material of sub products such as preparation molecular sieve; After first-time filtrate added scavenging agent SDD degree of depth removing heavy metals ion, carry out secondary filtration, washing; At last, the manganese sulfate solution that obtains is sent to the potroom preparing electrolyte.
Embodiment three:
Manganese-silicon slag ore deposit is finely ground to the breeze of mean particle size below 100 orders, gets 100g; Use and initially contain acid concentration and size mixing liquid-solid ratio 6: 1 as the sulphuric acid soln of 30/L; Slip after sizing mixing adds in the reaction vessel, and controlled temperature is at 85 ℃; The pH value of control solution is in certain scope in leaching process, and the reaction times is discharging behind 80min; Add a small amount of manganese alloy slag in the slip after going out reaction vessel, neutralize most spent acid, add among the proper C aO again and remaining a small amount of spent acid, regulate the pH value between 6.5 to 7; Filter washing then; The leached mud that obtains behind the filtration washing is as the raw material of sub products such as preparation molecular sieve; After first-time filtrate added scavenging agent SDD degree of depth removing heavy metals ion, carry out secondary filtration, washing; At last, the manganese sulfate solution that obtains is sent to the potroom preparing electrolyte.
Embodiment four:
Manganese-silicon slag ore deposit is finely ground to the breeze of mean particle size more than 100 orders, gets 100g; Use and initially contain acid concentration and size mixing liquid-solid ratio 5: 1 as the sulphuric acid soln of 10g/L; Slip after sizing mixing adds in the reaction vessel, and controlled temperature is at 90 ℃; The pH value of control solution is in certain scope in leaching process, and the reaction times is discharging behind 60min; Add a small amount of manganese alloy slag in the slip after going out reaction vessel, neutralize most spent acid, add among the proper C aO again and remaining a small amount of spent acid, regulate the pH value between 6.5 to 7; Filter washing then; The leached mud that obtains behind the filtration washing is as the raw material of sub products such as preparation molecular sieve; After first-time filtrate added scavenging agent SDD degree of depth removing heavy metals ion, carry out secondary filtration, washing; At last, the manganese sulfate solution that obtains is sent to the potroom preparing electrolyte.
Estimate for manganese alloy slag normal pressure of the present invention is leached the method effect of producing manganous sulfate, 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.
Manganese leaching yield=(1-C
1M
1/ M) * 100%
Wherein: M---manganese element total mass in the raw material; The g of unit;
C
1---the quality percentage composition of manganese element in the filter residue, the wt% of unit;
M
1---the quality of filter residue, the g of unit;
Slag rate=(M
1/ M
0) * 100%
Wherein: M
0---raw material ore deposit total mass; The g of unit;
M
1---the quality of filter residue, the g of unit;
Contain manganese=C in the leached mud
1M
1
Wherein: C
1---the quality percentage composition of manganese element in the filter residue, the wt% of unit;
M
1---the quality of filter residue, the g of unit;
Table 1
Can find out by table 1; Adopting method of the present invention that manganese alloy slag (carbon-manganese alloy slag and manganese-silicon slag) is carried out normal pressure leaches; The leaching yield of manganese all can realize more than 86%; 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 final realization manganese alloy slag reclaims.In addition, it is simple that the method that manganous sulfate is produced in this manganese alloy slag normal pressure leaching has technical process, the material low price, and production cost is low, and the treatment time is short, the advantage friendly to physical environment.
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 (10)
1. a manganese alloy slag normal pressure leaches the method for producing manganous sulfate, it is characterized in that, may further comprise the steps:
A) said manganeseirom slag is sized mixing with sulphuric acid soln, obtain mixed slurry;
B) said mixed slurry is added in the reaction vessel;
C) the pH value of control solution in reaction process, and discharging after the normal pressure acidleach obtains acidleach and goes out mixture; With
D) said acidleach is gone out mixture and carry out solid-liquid separation, obtain manganese sulfate solution.
2. manganese alloy slag normal pressure according to claim 1 leaches the method for producing manganous sulfate, it is characterized in that in the said step a), said manganese alloy slag is meant carbon-manganese alloy slag and manganese-silicon slag etc., and its granularity is controlled at more than 100 orders.
3. manganese alloy slag normal pressure according to claim 1 leaches the method for producing manganous sulfate, it is characterized in that in the said step a), the initial acidity of said sulphuric acid soln is 1g/L～100g/L, and the liquid-solid ratio in the said mixed slurry is 3: 1～16: 1.
4. manganese alloy slag normal pressure according to claim 1 leaches the method for producing manganous sulfate, it is characterized in that, in said step b), the temperature in the said reaction vessel is controlled at 50 ℃～98 ℃.
5. manganese alloy slag normal pressure according to claim 1 leaches the method for producing manganous sulfate, it is characterized in that in the said step c), the extraction time of said normal pressure acidleach is 60～120min.
6. manganese alloy slag normal pressure according to claim 1 leaches the method for producing manganous sulfate, it is characterized in that, may further comprise the steps in the said step d):
D-1) add manganese alloy slag and quicklime in the slip after going out reaction vessel, making its pH value is in 6.5～7 scopes so that neutralization acid wherein; With
D-2) slip after neutralizing treatment once filters, washs, and obtains manganous sulfate filtrating and leached mud.
7. manganese alloy slag normal pressure according to claim 6 leaches the method for producing manganous sulfate, it is characterized in that, with the raw material of said leached mud as the preparation molecular sieve.
8. manganese alloy slag normal pressure according to claim 6 leaches the method for producing manganous sulfate, it is characterized in that said step d) further comprises:
D-3) in said manganous sulfate filtrating, add scavenging agent, carry out secondary filtration, washing, obtain the high-purity sulphuric acid manganese solution with after removing heavy metal ion wherein.
9. manganese alloy slag normal pressure according to claim 8 leaches the method for producing manganous sulfate, it is characterized in that said scavenging agent is a Sodium Dimethyldithiocarbamate.
10. leach the method for producing manganous sulfate according to each described manganese alloy slag normal pressure in the claim 6～9, it is characterized in that vacuum filtration method or filter press technique are adopted in said filtration.
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| CN201110306177 | 2011-10-10 | ||
| CN201110305075.7 | 2011-10-10 | ||
| CN201110305135.5 | 2011-10-10 | ||
| CN2011103051355A CN102367515A (en) | 2011-10-10 | 2011-10-10 | Pressurizing and reductive leaching method of pyrolusite powder |
| CN2011103050757A CN102367521A (en) | 2011-10-10 | 2011-10-10 | Method for leaching of manganese from manganese-containing smelt flue dust |
| CN201110305124.7 | 2011-10-10 | ||
| CN201110305124 | 2011-10-10 | ||
| CN201110306177.0 | 2011-10-10 | ||
| CN2012101184287A CN102618728A (en) | 2011-10-10 | 2012-04-20 | Method for producing manganese sulfate by leaching manganese alloy slag under normal pressure |
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| CN201210118398XA Pending CN102605188A (en) | 2011-10-10 | 2012-04-20 | Method for producing manganese sulfate by manganese alloy slag through pressure leaching |
| CN2012101183566A Pending CN102605186A (en) | 2011-10-10 | 2012-04-20 | Method for producing manganese sulfate from manganese-rich slag through atmospheric pressure leaching |
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| CN102094119A (en) * | 2011-01-21 | 2011-06-15 | 吉首大学 | Method for preparing electrolytic manganese metal with low-grade pyrolusite wet leaching |
| CN102220491A (en) * | 2011-06-03 | 2011-10-19 | 郭永锴 | Method for recovering manganese from manganese ore, manganese tailing and manganese slag through continuous pressurization and acid leaching process |
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2012
- 2012-04-20 CN CN2012101183886A patent/CN102605187A/en active Pending
- 2012-04-20 CN CN201210118398XA patent/CN102605188A/en active Pending
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| CN1960796A (en) * | 2004-05-25 | 2007-05-09 | 费罗兰特卡有限公司 | Method of obtaining electrolytic manganese from ferroalloy production waste |
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| CN107287430A (en) * | 2017-08-29 | 2017-10-24 | 铜仁学院 | A kind of method for extracting manganese in electrolytic manganese residues and the method for handling electrolytic manganese residues |
| CN107299226A (en) * | 2017-08-29 | 2017-10-27 | 铜仁学院 | A kind of method of Microwave Extraction manganese in electrolytic manganese residues |
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| CN102605187A (en) | 2012-07-25 |
| CN102605188A (en) | 2012-07-25 |
| CN102605186A (en) | 2012-07-25 |
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