CN104294038A - Technology for preparing manganese carbonate from silver-manganese ores - Google Patents
Technology for preparing manganese carbonate from silver-manganese ores Download PDFInfo
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Abstract
The invention relates to a technology for preparing manganese carbonate from silver-manganese ores. The manganese leaching rate of the technology is greater than 98%, and the later stage silver leaching rate can reach 95%; Fe in a manganese leaching liquid can be completely removed through pre-oxidation and an E.Z. goethite process, and the Fe content in the iron removed liquid is less than 1mg/L, so the iron removal rate reaches 99.99%; heavy meal impurities in the manganese leaching liquid can be removed through a sulfuration process, and the removal rates of Co, Ni and Zn reach 97.19%, 99.84% and 72.10% respectively, so the purifying effect is good; and a manganese carbonate product is successfully prepared, and the quality of the product reaches requirements of one-grade products.
Description
Technical field
The present invention relates to manganous carbonate and produce field, be specifically related to a kind of technique producing manganous carbonate from silver-colored manganese ore.
Background technology
In recent years, divide all in succession found silver-colored manganese ore deposit in many provinces of China, the Fe content in these mineral deposits is generally at 10%-30%, and the grade of silver is at 150g/t to a few kg/t.The silver-colored manganese ore reserves that China is verified have reached thousands of tons of (in argent), but not yet solve due to selecting and smelting technology problem, and this kind of ore of China not yet obtains effective development and utilization.Manganese in silver-manganese ore is the oxide mineral such as pyrolusite, psilomelane mainly, main existence form is MnO2, MnS, the silver mineral of its association mainly exists with forms such as native silver, kustelite, electrum, composing in isomorph mode in fine particle is stored in manganese ore lattice, both the mode being difficult to be sorted by machinery obtains high-grade silver preparation concentrate, also be difficult to obtain silver preferably by single cyanide process and leach index, be acknowledged as unmanageable containing one of silver ore, silver-colored manganese ore treatment process research is also subject to domestic and international common concern.
The process of current stage to silver-colored manganese ore mainly contains pyrogenic process and the large class of wet method two.Pyrogenic process mainly contains blast-furnace smelting method and reducing roasting lixiviation process.Wet method can be divided into again two-step approach, single stage method and Bioleaching method three major types.The two-step approach of report is wherein had to have using sulfur dioxide reduction method, two-control region, ferrous sulfate method, aniline process etc.Single stage method has thiosulfate technique, sour sulfur pulpating method, hydrogen peroxide method etc.
In actual applications thermal process because energy consumption is high, environmental pollution is serious and metal recovery rate is low is not widely adopted.Manganese, silver can leach in solution by the single stage method in wet processing simultaneously, the shortcomings such as technical process is short, but there is operational condition harshness, poor stability, and later separation is complicated, oneself rests on experimental stage, the domestic report there are no industrial application by the document of report mostly.Bioleaching method is the novel method that external silver-colored manganese is separated, and has the advantage that reagent consumption amount is few, free from environmental pollution, but also there is the defect that leaching velocity is slow, the operational cycle is long.Current stage silver manganese ore main methods be two-step approach, wherein comparative maturity is sulfurous gas method and two-control region.
China studies for manganese oxide ore (MnO2), is also all used to Processing Ag manganese oxide ore in the treatment process of above-mentioned silver-colored manganese ore.And the method that the silver-colored manganese ore that the major ingredient of silver-colored manganese is sulphide ores produces silver-colored manganese ore leaching manganese liquid document at home and abroad does not all also have similar report.
Manganous carbonate is a kind of general material of having many uses, and it may be used for: (1) manufactures soft magnetic ferrite.Manganous carbonate was once the main raw material that soft magnetic ferrite is produced, but nearly ten years, the production of soft magnetic ferrite progressively adopts trimanganese tetroxide to substitute manganous carbonate, and manganous carbonate has the trend be eliminated in this field; (2) manufacture the raw material of other manganese salt, be mainly used for producing chemical mno2; (3) pigment of coating and paint; (4) production of mangal and manganese-silicon; (5) fertilizer and fodder additives; (6) paint drier; (7) the multiple material of welding electrode; (8) pharmacy etc.
The production of China's manganous carbonate be mostly with rhodochrosite and pyrolusite for raw material, prepare manganous carbonate with the leaching manganese liquid of silver-colored manganese ore as raw material and also do not seen same process report.
Therefore, the major ingredient that the present invention is directed to silver-colored manganese is that the method that the silver-colored manganese ore of sulphide ores produces silver-colored manganese ore leaching manganese liquid is studied, and prepared manganous carbonate by the leaching manganese liquid of silver-colored manganese ore as raw material, being conducive to is utilization and the exploitation of the silver-colored manganese ore of sulphide ores to the major ingredient of silver-colored manganese.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to provide a kind of technique producing manganous carbonate from silver-colored manganese ore.The leaching yield of described technique manganese is greater than 98%, and the leaching yield of later stage silver can reach 95%; Can the Fe in leaching manganese liquid be removed clean by preoxidation and E.Z. separation of iron in goethite form, the Fe after deironing in liquid
t<1mg/L, deironing rate is up to 99.99%; Adopt sulfuration method can remove beavy metal impurity in leaching manganese liquid, wherein the purification rate of Co, Ni, Zn reaches 97.19%, 99.84%, 72.10% respectively, and decontamination effect improving is good; Successfully prepared manganese carbonate product, quality product reaches the requirement of first grade.
Present invention employs following technical scheme:
From silver-colored manganese ore, produce a technique for manganous carbonate, it comprises the following steps:
Producing of silver manganese ore leaching manganese liquid: adopt pyrolusite (MnO2) to make oxygenant, at sulfuric acid 3.5-4.5N, catalyzer 0.35-0.45N, liquid-solid ratio L/S=2.5-3.5, pyrolusite amount is the 35-45% of silver-colored manganic concerntrate, temperature 85-95 DEG C, leaches under the condition of time 1.5-2.5h;
Neutralization: adopt rhodochrosite (MnCO3) to make neutralizing agent, the sulfuric acid at 75-85 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1;
E.Z. separation of iron in goethite form: add pyrolusite oxidation of ferrous iron to ferric iron at 75-85 DEG C; Adopt lime to carry out as neutralizing agent, terminal pH=5-6, is incubated 0.5-1 hour after reaction is reached home;
Sulfuration method removing heavy metals: adopt diethyldithiocarbamate to remove beavy metal impurity in leaching manganese liquid as precipitation agent sulfuration method at 55-65 DEG C;
Produce manganous carbonate: adopt bicarbonate of ammonia to make precipitation agent, add the bicarbonate of ammonia of theoretical amount 1.2 times; The starting point concentration of bicarbonate of ammonia is 75-85g/L; Unsuitable too high about 30 DEG C of the temperature of reaction; The pH value of reaction end should control at about 6.5-7.5.
Wherein preferred technique is:
Producing of silver manganese ore leaching manganese liquid: adopt pyrolusite (MnO2) to make oxygenant, at sulfuric acid 4N, catalyzer 0.4N, liquid-solid ratio L/S=3, pyrolusite amount is 40% of silver-colored manganic concerntrate, and temperature 90 DEG C, leaches under the condition of time 2h;
Neutralization: adopt rhodochrosite (MnCO3) to make neutralizing agent, the sulfuric acid at 80 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1.
E.Z. separation of iron in goethite form: add pyrolusite oxidation of ferrous iron to ferric iron at 80 DEG C; Adopt lime to carry out as neutralizing agent, terminal pH=5.5, is incubated 45min after reaction is reached home.
Sulfuration method removing heavy metals: adopt diethyldithiocarbamate to remove beavy metal impurity in leaching manganese liquid as precipitation agent sulfuration method at 60 DEG C.
Produce manganous carbonate: adopt bicarbonate of ammonia to make precipitation agent, add the bicarbonate of ammonia of theoretical amount 1.2 times; The starting point concentration of bicarbonate of ammonia is 79g/L; Unsuitable too high about 30 DEG C of the temperature of reaction; The pH value of reaction end should control about 7.
Wherein, described silver-colored manganese ore is the silver floatation manganese ore concentrate of Guangxi phoenix silver ore.
Wherein, the Chemical Composition of described silver-colored manganese ore comprises (wt%): 0.796Ag, 4.31Pb, 3.08Zn, 0.24Cu, 10.97As, 23.46S, 18.09Fe, 17.29Mn.
The present invention has the following advantages:
(1) pyrolusite (MnO2) is adopted to make oxygenant, at sulfuric acid 4N, catalyzer 0.4N, liquid-solid ratio L/S=3, pyrolusite amount is 40% of silver-colored manganic concerntrate, temperature 90 DEG C, under the condition of time 2h, in silver-colored manganese ore, the leaching yield of manganese is greater than 98%, and the leaching yield of later stage silver can reach 95%.
(2) soaking sulfuric acid content higher (83.17g/L) in manganese liquid adopts rhodochrosite (MnCO3) to make neutralizing agent, and the sulfuric acid at 80 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1.
(3) systematic research has been carried out to the technique of E.Z. separation of iron in goethite form, can the Fe in leaching manganese liquid removed clean by preoxidation and E.Z. separation of iron in goethite form.Fe after deironing in liquid
t<1mg/L, deironing rate is up to 99.99%.
(4) sulfuration method is adopted can to remove beavy metal impurity in leaching manganese liquid.Wherein the purification rate of Co, Ni, Zn reaches 97.19%, 99.84%, 72.10% respectively, and decontamination effect improving is good.
(5) successfully prepared manganese carbonate product, quality product reaches the requirement of first grade.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment one
From silver-colored manganese ore, produce a technique for manganous carbonate, it comprises the following steps:
Producing of silver manganese ore leaching manganese liquid: adopt pyrolusite (MnO2) to make oxygenant, at sulfuric acid 4N, catalyzer 0.4N, liquid-solid ratio L/S=3, pyrolusite amount is 40% of silver-colored manganic concerntrate, and temperature 90 DEG C, leaches under the condition of time 2h;
Neutralization: adopt rhodochrosite (MnCO3) to make neutralizing agent, the sulfuric acid at 80 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1.
E.Z. separation of iron in goethite form: add pyrolusite oxidation of ferrous iron to ferric iron at 80 DEG C; Adopt lime to carry out as neutralizing agent, terminal pH=5.5, is incubated 45min after reaction is reached home.
Sulfuration method removing heavy metals: adopt diethyldithiocarbamate to remove beavy metal impurity in leaching manganese liquid as precipitation agent sulfuration method at 60 DEG C.
Produce manganous carbonate: adopt bicarbonate of ammonia to make precipitation agent, add the bicarbonate of ammonia of theoretical amount 1.2 times; The starting point concentration of bicarbonate of ammonia is 79g/L; Unsuitable too high about 30 DEG C of the temperature of reaction; The pH value of reaction end should control about 7.
Wherein, the Chemical Composition of described silver-colored manganese ore comprises (wt%): 0.796Ag, 4.31Pb, 3.08Zn, 0.24Cu, 10.97As, 23.46S, 18.09Fe, 17.29Mn.
Embodiment two
From silver-colored manganese ore, produce a technique for manganous carbonate, it comprises the following steps:
Producing of silver manganese ore leaching manganese liquid: adopt pyrolusite (MnO2) to make oxygenant, at sulfuric acid 3.5N, catalyzer 0.35N, liquid-solid ratio L/S=2.5, pyrolusite amount is 35% of silver-colored manganic concerntrate, and temperature 85 DEG C, leaches under the condition of time 1.5h;
Neutralization: adopt rhodochrosite (MnCO3) to make neutralizing agent, the sulfuric acid at 75 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1;
E.Z. separation of iron in goethite form: add pyrolusite oxidation of ferrous iron to ferric iron at 75 DEG C; Adopt lime to carry out as neutralizing agent, terminal pH=5, after reaction is reached home, be incubated 0.5 hour;
Sulfuration method removing heavy metals: adopt diethyldithiocarbamate to remove beavy metal impurity in leaching manganese liquid as precipitation agent sulfuration method at 55 DEG C;
Produce manganous carbonate: adopt bicarbonate of ammonia to make precipitation agent, add the bicarbonate of ammonia of theoretical amount 1.2 times; The starting point concentration of bicarbonate of ammonia is 75g/L; Unsuitable too high about 30 DEG C of the temperature of reaction; The pH value of reaction end should control about 6.5.
Wherein, the Chemical Composition of described silver-colored manganese ore comprises (wt%): 0.796Ag, 4.31Pb, 3.08Zn, 0.24Cu, 10.97As, 23.46S, 18.09Fe, 17.29Mn.
Embodiment three
From silver-colored manganese ore, produce a technique for manganous carbonate, it comprises the following steps:
Producing of silver manganese ore leaching manganese liquid: adopt pyrolusite (MnO2) to make oxygenant, at sulfuric acid 4.5N, catalyzer 0.45N, liquid-solid ratio L/S=3.5, pyrolusite amount is 45% of silver-colored manganic concerntrate, and temperature 95 DEG C, leaches under the condition of time 2.5h;
Neutralization: adopt rhodochrosite (MnCO3) to make neutralizing agent, the sulfuric acid at 85 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1;
E.Z. separation of iron in goethite form: add pyrolusite oxidation of ferrous iron to ferric iron at 85 DEG C; Adopt lime to carry out as neutralizing agent, terminal pH=6, after reaction is reached home, be incubated 1 hour;
Sulfuration method removing heavy metals: adopt diethyldithiocarbamate to remove beavy metal impurity in leaching manganese liquid as precipitation agent sulfuration method at 65 DEG C;
Produce manganous carbonate: adopt bicarbonate of ammonia to make precipitation agent, add the bicarbonate of ammonia of theoretical amount 1.2 times; The starting point concentration of bicarbonate of ammonia is 85g/L; Unsuitable too high about 30 DEG C of the temperature of reaction; The pH value of reaction end should control about 7.5.
Wherein, the Chemical Composition of described silver-colored manganese ore comprises (wt%): 0.796Ag, 4.31Pb, 3.08Zn, 0.24Cu, 10.97As, 23.46S, 18.09Fe, 17.29Mn.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (8)
1. from silver-colored manganese ore, produce a technique for manganous carbonate, it comprises the following steps:
Producing of silver manganese ore leaching manganese liquid: adopt pyrolusite (MnO2) to make oxygenant, at sulfuric acid 3.5-4.5N, catalyzer 0.35-0.45N, liquid-solid ratio L/S=2.5-3.5, pyrolusite amount is the 35-45% of silver-colored manganic concerntrate, temperature 85-95 DEG C, leaches under the condition of time 1.5-2.5h;
Neutralization: adopt rhodochrosite (MnCO3) to make neutralizing agent, the sulfuric acid at 75-85 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1;
E.Z. separation of iron in goethite form: add pyrolusite oxidation of ferrous iron to ferric iron at 75-85 DEG C; Adopt lime to carry out as neutralizing agent, terminal pH=5-6, is incubated 0.5-1 hour after reaction is reached home;
Sulfuration method removing heavy metals: adopt diethyldithiocarbamate to remove beavy metal impurity in leaching manganese liquid as precipitation agent sulfuration method at 55-65 DEG C;
Produce manganous carbonate: adopt bicarbonate of ammonia to make precipitation agent, add the bicarbonate of ammonia of theoretical amount 1.2 times; The starting point concentration of bicarbonate of ammonia is 75-85g/L; Unsuitable too high about 30 DEG C of the temperature of reaction; The pH value of reaction end should control at about 6.5-7.5.
2. technique according to claim 1, producing of preferred silver-colored manganese ore leaching manganese liquid: adopt pyrolusite (MnO2) to make oxygenant, at sulfuric acid 4N, catalyzer 0.4N, liquid-solid ratio L/S=3, pyrolusite amount is 40% of silver-colored manganic concerntrate, temperature 90 DEG C, leaches under the condition of time 2h.
3. technique according to claim 1, preferably neutralizes: adopt rhodochrosite (MnCO3) to make neutralizing agent, and the sulfuric acid at 80 DEG C and in leaching manganese liquid, the add-on of its manganese carbonate ore, controls with terminal pH=1.
4. technique according to claim 1, preferred E.Z. separation of iron in goethite form: add pyrolusite oxidation of ferrous iron to ferric iron at 80 DEG C; Adopt lime to carry out as neutralizing agent, terminal pH=5.5, is incubated 45min after reaction is reached home.
5. technique according to claim 1, preferred sulfuration method removing heavy metals: adopt diethyldithiocarbamate to remove beavy metal impurity in leaching manganese liquid as precipitation agent sulfuration method at 60 DEG C.
6. technique according to claim 1, preferably produces manganous carbonate: adopt bicarbonate of ammonia to make precipitation agent, add the bicarbonate of ammonia of theoretical amount 1.2 times; The starting point concentration of bicarbonate of ammonia is 79g/L; Unsuitable too high about 30 DEG C of the temperature of reaction; The pH value of reaction end should control about 7.
7. technique according to claim 1, wherein, described silver-colored manganese ore is the silver floatation manganese ore concentrate of Guangxi phoenix silver ore.
8. technique according to claim 1, wherein, the Chemical Composition of described silver-colored manganese ore comprises (wt%): 0.796Ag, 4.31Pb, 3.08Zn, 0.24Cu, 10.97As, 23.46S, 18.09Fe, 17.29Mn.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119565A (en) * | 2016-06-22 | 2016-11-16 | 湖南大学 | A kind of method that leaching of manganese and silver produce manganese sulfate and silver from manganese-silver ore |
| CN106367589A (en) * | 2016-09-19 | 2017-02-01 | 北京科技大学 | Short-process low-consumption high-purity manganese sulfate solution preparing method |
| CN106395910A (en) * | 2016-08-29 | 2017-02-15 | 中南大学 | Method for preparation of battery grade high-purity manganese sulfate from industrial grade manganese sulfate |
| CN106673066A (en) * | 2016-11-11 | 2017-05-17 | 中南大学 | Preparation method of high-purity anhydrous manganese chloride particles |
| CN107117657A (en) * | 2017-06-23 | 2017-09-01 | 中南大学 | The method that high-pure anhydrous manganese chloride is prepared using technical grade sulfuric acid manganese |
| CN108660326A (en) * | 2018-05-25 | 2018-10-16 | 东北大学 | A method of reduction acidolysis-leaching is simultaneously except iron handles manganese oxide ore |
| CN111286603A (en) * | 2020-03-25 | 2020-06-16 | 内蒙古金山矿业有限公司 | Process for recovering silver and co-producing manganese sulfate from manganese-containing silver ore |
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2013
- 2013-07-19 CN CN201310307635.1A patent/CN104294038A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119565A (en) * | 2016-06-22 | 2016-11-16 | 湖南大学 | A kind of method that leaching of manganese and silver produce manganese sulfate and silver from manganese-silver ore |
| CN106395910A (en) * | 2016-08-29 | 2017-02-15 | 中南大学 | Method for preparation of battery grade high-purity manganese sulfate from industrial grade manganese sulfate |
| CN106367589A (en) * | 2016-09-19 | 2017-02-01 | 北京科技大学 | Short-process low-consumption high-purity manganese sulfate solution preparing method |
| CN106673066A (en) * | 2016-11-11 | 2017-05-17 | 中南大学 | Preparation method of high-purity anhydrous manganese chloride particles |
| CN107117657A (en) * | 2017-06-23 | 2017-09-01 | 中南大学 | The method that high-pure anhydrous manganese chloride is prepared using technical grade sulfuric acid manganese |
| CN108660326A (en) * | 2018-05-25 | 2018-10-16 | 东北大学 | A method of reduction acidolysis-leaching is simultaneously except iron handles manganese oxide ore |
| CN111286603A (en) * | 2020-03-25 | 2020-06-16 | 内蒙古金山矿业有限公司 | Process for recovering silver and co-producing manganese sulfate from manganese-containing silver ore |
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Application publication date: 20150121 |