CN103451673A - Production method of electrolytic manganese metal - Google Patents
Production method of electrolytic manganese metal Download PDFInfo
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- CN103451673A CN103451673A CN2013103446306A CN201310344630A CN103451673A CN 103451673 A CN103451673 A CN 103451673A CN 2013103446306 A CN2013103446306 A CN 2013103446306A CN 201310344630 A CN201310344630 A CN 201310344630A CN 103451673 A CN103451673 A CN 103451673A
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Abstract
The invention discloses a production method of electrolytic manganese metal. The production method comprises the following steps of milling, slurrying, leaching oxidizing, neutralizing, primary filter pressing, secondary filter pressing, electrolyzing, out-of-tank passivating, flushing, drying and stripping. Due to the addition of the slurrying step, raw ore powder is caused to react thoroughly in a quite mild chemical environment (45 to 50 DEG C) and then the extraction speed and the extraction rate of manganese are greatly increased; an anode liquor does not need to be heated near boiling by introducing steam and the like, so that the heat source cost is greatly saved; by comparing the new and old two production lines in the factory of the applicant of the invention, the fuel cost or electric charge can be saved by using the method provided by the invention. In the meantime, air oxidization is applied to remove iron instead of iron removal through manganese dioxide in a traditional process; for producing one ton of manganese, the manganese dioxide powder can be saved; consequently, the production cost is further reduced.
Description
Technical field
The present invention relates to a kind of production method of electrolytic manganese, particularly a kind of production method of energy-efficient electrolytic metal Mn.
Background technology
Manganese is indispensable additive in metallurgy industry, electrolytic manganese is the main raw material of producing trimanganese tetroxide after being processed into powdery, the widely used magneticsubstance original paper of electronic industry is produced with trimanganese tetroxide, and electronic industry, metallurgical industry and aerospace industry all need electrolytic metal Mn.Along with improving constantly of scientific and technical development and the level of the productive forces; electrolytic metal Mn, due to its high purity, low impurity characteristics, now successfully applies to the every field such as smelting iron and steel, nonferrous metallurgy, electronic technology, chemical industry, environment protection, food sanitation, welding electrode industry, space industry widely.
The production method of manganese metal has two kinds.A kind of is to adopt electrolytic process, and products obtained therefrom is electrolytic metal Mn; Another kind is that to take rich manganese ore and high silicon manganese-silicon alloy be raw material, by electric furnace desiliconization purifying method, produces, and product claims manganese metal.The manganese carbonate ore that electrolytic process Chang Yihan manganese is lower is raw material, through broken, be finely ground to breeze, add and be equipped with in the leaching can that returns to anolyte, add sulfuric acid, pass into steam heating and be bordering on boiling, make the manganese leaching in breeze enter solution, add appropriate buffer reagent ammonium sulfate, and add the manganese dioxide powder deironing in acid ore pulp, then pass into liquefied ammonia or add milk of lime to make ore pulp become neutral (pH ≈ 7), solid-liquid separation is removed residue, toward add in filtrate vulcanizing agent (the dimethyl amine nabam, (CH3)
2nCS
2na, be called for short SDD) or diethyldithiocarbamate purify, make nickel, cobalt, iron plasma sulphidisation form Precipitation, remove vulcanized slag through solid-liquid separation for the second time, add additive (SeO
2or SO
2), obtain qualified electrolytic solution.During electrolysis, qualified electrolytic solution continuously adds electrolyzer, through the energising electrolysis to certain hour (being generally 24h), take out with the negative plate of galvanic deposit manganese and (put into clean negative plate simultaneously, electrolysis is carried out continuously), after passivation, washing, oven dry, manganese metal is peeled, be finished product.The existing electrolytic metal Mn industrial scale of China is generally less, reaches 5000t large every year, and little often is only hundreds of tons.And the employing traditional technology, except front operation liquid mode processed is not quite similar, electrolysis production technique is basic identical.Its maximum shortcoming is that energy consumption is high, and manganese recovery ratio is undesirable.
For above-mentioned deficiency, need to be optimized improvement to existing electrolytic manganese process, to adapt to large-scale production, the while is energy efficient greatly, reduces costs, and improves greatly the rate of recovery of manganese metal.
Summary of the invention
In view of this, the invention provides a kind of energy-conservation, efficient and cost-saving electrolytic manganese production method.
The present invention solves the problems of the technologies described above by following technique means: a kind of production method of electrolytic metal Mn comprises the following steps:
A, powder process: raw ore is crushed to 90-100 orders;
B, pulp: the proportioning that breeze prepared by steps A and anolyte are 1:3 according to the solid-to-liquid ratio chemical combination bucket of packing into, fully be uniformly mixed, wherein in anolyte, the content concn of Mn is 11-14g/l, the H content concn is 38-45g/l; Then under the temperature environment of 45 ℃-50 ℃, react 10-20 minutes; Add the sulfuric acid that is equivalent to breeze weight 40%, the concentration of sulfuric acid is 98% again, Leaching reaction 4-6 hours, and spent acid concentration is controlled at 0.9g/L-1.5g/L;
C, leach oxidation: pass into air in the chemical combination bucket, accelerated reaction, more than 60 minutes, utilizes airborne dioxygen oxidation deironing;
D, neutralization: add the ammoniacal liquor that concentration is 11%-15% that pH value is adjusted to 6.4, continue to keep, more than 30 minutes, to add the Sodium Dimethyldithiocarbamate removal heavy metal;
E, a press filtration: become sulfuration liquid through thick the pressure, in filter residue, the moisture content massfraction is controlled in 23%, and in filter residue, the massfraction of manganese is in 2%;
F, secondary press filtration: become qualifying liquid through the secondary press filtration again;
G, electrolysis: electrolysing period is 24 hours, groove temperature 40-46 degree, pH value is between 6.8-7.4;
H, go out the groove passivation, rinses product to without sulphur-cake, then dry, peel off and get final product.
Further, in step B, in anolyte, the content concn of Mn is 13g/l, and the H content concn is 40g/l; Then under the temperature environment of 48 ℃, react 18 minutes; Add the sulfuric acid that is equivalent to breeze weight 40%, the concentration of sulfuric acid is 96% again, Leaching reaction 5 hours, and spent acid concentration is controlled at 1.0g/L-1.1g/L.
Further, in steps A, adopt Vertical Mill negative pressure powder-making machine to carry out powder process.
Further, in step e and step F, described filtering equipment adopts high pressure eardrum pressure filter.
Further, in step G, the electrolyzer that adopts is made by the RPP material.
Further, in step H, adopt ultrasonic wave to wash plate and washed plate.
Beneficial effect of the present invention: the production method of electrolytic metal Mn of the present invention, with the production method of traditional electrolytic metal Mn, compare, there is following beneficial effect:
1, owing to having increased the pulp step, make original ore powder (45 ℃-50 ℃) under comparatively gentle chemical environment that fully reaction occur, accelerated greatly speed and eduction rate that manganese is separated out; Without passing into steam etc., the anolyte heating is bordering on to boiling, has greatly saved the thermal source cost, by two new and old production lines contrasts of the applicant's factory, adopt this processing method to produce 500-600 yuan of one ton of manganese ore cost capable of saving fuel or the electricity charge.Adopt the atmospheric oxidation deironing simultaneously, replace the Manganse Dioxide deironing of traditional technology, produce manganese per ton and can save the manganese dioxide powder of 150-180 yuan, further reduced production cost.
2, in the electrolytic manganese production industry, first adopts Vertical Mill negative pressure powder manufacturing apparatus, has effectively stopped dust pollution, with traditional powder manufacturing apparatus, compares, and product breeze per ton 25-30 degree that can economize on electricity, convert as Electrolytic Manganese Product economize on electricity per ton 250 degree left and right.
3, attempt first adopting the energy-conservation electrolyzer of RPP material in the electrolytic manganese industry, facts have proved that product per ton can economize on electricity about 600 degree.
4, adopt high pressure eardrum pressure filter, manganese slag water content is reduced in 23% from traditional 30% left and right, has greatly improved manganese recovery ratio.
5, adopt ultrasonic wave to wash plate and wash product, the sump consumption is reduced in 0.3m3 from tradition product 3m3 per ton, nearly 30,000 m3 of annual water-saving amount.
Embodiment
Embodiment 1
A kind of production method of electrolytic metal Mn comprises the following steps:
A, powder process: raw ore is crushed to 90 orders;
B, pulp: the proportioning that breeze prepared by steps A and anolyte are 1:3 according to the solid-to-liquid ratio chemical combination bucket of packing into, fully be uniformly mixed, wherein in anolyte, the content concn of Mn is 14g/l, the H content concn is 38g/l; Then under the temperature environment of 50 ℃, react 10 minutes; Add the sulfuric acid that is equivalent to breeze weight 40%, the concentration of sulfuric acid is 98% again, Leaching reaction 6 hours, and spent acid concentration is controlled at 0.9g/L;
C, leach oxidation: pass into air in the chemical combination bucket, accelerated reaction, more than 60 minutes, utilizes airborne dioxygen oxidation deironing;
D, neutralization: add the ammoniacal liquor that concentration is 15% that pH value is adjusted to 6.4, continue to keep, more than 30 minutes, to add the Sodium Dimethyldithiocarbamate removal heavy metal;
E, a press filtration: become sulfuration liquid through thick the pressure, in filter residue, the moisture content massfraction is controlled in 23%, and in filter residue, the massfraction of manganese is in 2%;
F, secondary press filtration: become qualifying liquid through the secondary press filtration again;
G, electrolysis: electrolysing period is 24 hours, groove temperature 40 degree, pH value is 7.4;
H, go out the groove passivation, rinses product to without sulphur-cake, then dry, peel off and get final product.
Embodiment 2
A kind of production method of electrolytic metal Mn comprises the following steps:
A, powder process: raw ore is crushed to 100 orders;
B, pulp: the proportioning that breeze prepared by steps A and anolyte are 1:3 according to the solid-to-liquid ratio chemical combination bucket of packing into, fully be uniformly mixed, wherein in anolyte, the content concn of Mn is 11g/l, the H content concn is 45g/l; Then under the temperature environment of 45 ℃, react 20 minutes; Add the sulfuric acid that is equivalent to breeze weight 40%, the concentration of sulfuric acid is 96% again, Leaching reaction 4 hours, and spent acid concentration is controlled at 1.5g/L;
C, leach oxidation: pass into air in the chemical combination bucket, accelerated reaction, more than 60 minutes, utilizes airborne dioxygen oxidation deironing;
D, neutralization: add the ammoniacal liquor that concentration is 11% that pH value is adjusted to 6.4, continue to keep, more than 30 minutes, to add the Sodium Dimethyldithiocarbamate removal heavy metal;
E, a press filtration: become sulfuration liquid through thick the pressure, in filter residue, the moisture content massfraction is controlled in 23%, and in filter residue, the massfraction of manganese is in 2%;
F, secondary press filtration: become qualifying liquid through the secondary press filtration again;
G, electrolysis: electrolysing period is 24 hours, groove temperature 46 degree, pH value is 6.8;
H, go out the groove passivation, rinses product to without sulphur-cake, then dry, peel off and get final product.
Embodiment 3
A kind of production method of electrolytic metal Mn comprises the following steps:
A, powder process: raw ore is crushed to 95 orders;
B, pulp: the proportioning that breeze prepared by steps A and anolyte are 1:3 according to the solid-to-liquid ratio chemical combination bucket of packing into, fully be uniformly mixed, wherein in anolyte, the content concn of Mn is 13g/l, the H content concn is 40g/l; Then under the temperature environment of 48 ℃, react 18 minutes; Add the sulfuric acid that is equivalent to breeze weight 40%, the concentration of sulfuric acid is 96% again, Leaching reaction 5 hours, and spent acid concentration is controlled at 1.0g/L or 1.1g/L;
C, leach oxidation: pass into air in the chemical combination bucket, accelerated reaction, more than 60 minutes, utilizes airborne dioxygen oxidation deironing;
D, neutralization: add the ammoniacal liquor that concentration is 13% that pH value is adjusted to 6.4, continue to keep, more than 30 minutes, to add the Sodium Dimethyldithiocarbamate removal heavy metal;
E, a press filtration: become sulfuration liquid through thick the pressure, in filter residue, the moisture content massfraction is controlled in 23%, and in filter residue, the massfraction of manganese is in 2%;
F, secondary press filtration: become qualifying liquid through the secondary press filtration again;
G, electrolysis: electrolysing period is 24 hours, groove temperature 42 degree, pH value is 7.0;
H, go out the groove passivation, rinses product to without sulphur-cake, then dry, peel off and get final product.
By the new and old two electrolytic manganese production lines practice of this factory, contrast: owing to having increased the pulp step, make original ore powder (45 ℃-50 ℃) under comparatively gentle chemical environment that fully reaction occur, accelerated greatly speed and eduction rate that manganese is separated out; Without passing into steam etc., the anolyte heating is bordering on to boiling, has greatly saved the thermal source cost, adopt the design parameter of above-mentioned three embodiment, produce 500-600 yuan of one ton of manganese ore cost capable of saving fuel or the electricity charge.Adopt the atmospheric oxidation deironing simultaneously, replace the Manganse Dioxide deironing of traditional technology, produce manganese per ton and can save the manganese dioxide powder of 150-180 yuan, further reduced production cost.In addition, the production cycle can shorten 3-4 hours, and production efficiency improves greatly.
As the further improvement to above-described embodiment, in steps A, adopt Vertical Mill negative pressure powder-making machine to carry out powder process.Effectively stopped dust pollution, compared with traditional powder manufacturing apparatus, product breeze per ton 25-30 degree that can economize on electricity, convert as Electrolytic Manganese Product economize on electricity per ton 250 degree left and right.
As the further improvement to above-described embodiment, in step e and step F, described filtering equipment adopts high pressure eardrum pressure filter.Adopt high pressure eardrum pressure filter, manganese slag water content is reduced in 23% from traditional 30% left and right, has greatly improved manganese recovery ratio.
As the further improvement to above-described embodiment, in step G, the electrolyzer that adopts is made by the RPP material.Attempt first adopting the energy-conservation electrolyzer of RPP material in the electrolytic manganese industry, facts have proved that product per ton can economize on electricity about 600 degree.
As the further improvement to above-described embodiment, in step H, adopt ultrasonic wave to wash plate and washed plate.Adopt ultrasonic wave to wash plate and wash product, the sump consumption is reduced in 0.3m3 from tradition product 3m3 per ton, nearly 30,000 m3 of annual water-saving amount.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not breaking away from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (6)
1. the production method of an electrolytic metal Mn is characterized in that: comprise the following steps:
A, powder process: raw ore is crushed to 90-100 orders;
B, pulp: the proportioning that breeze prepared by steps A and anolyte are 1:3 according to the solid-to-liquid ratio pulp bucket of packing into, be delivered to the chemical combination bucket after fully being uniformly mixed, under the temperature environment of 45 ℃-50 ℃, react 10-20 minutes; Add the sulfuric acid that is equivalent to breeze weight 40%, the concentration of sulfuric acid is 96%; And then add anolyte, and wherein in anolyte, the content concn of Mn is 11-14g/l, the H content concn is 38-45g/l; Leaching reaction 4-6 hours, spent acid concentration is controlled at 0.9g/L-1.5g/L;
C, leach oxidation: pass into air in the chemical combination bucket, accelerated reaction, more than 60 minutes, utilizes airborne dioxygen oxidation deironing;
D, neutralization: add the ammoniacal liquor that concentration is 11%-15% that pH value is adjusted to 6.4, continue to keep, more than 30 minutes, to add the Sodium Dimethyldithiocarbamate removal heavy metal;
E, a press filtration: become sulfuration liquid through thick the pressure, in filter residue, the moisture content massfraction is controlled in 23%, and in filter residue, the massfraction of manganese is in 2%;
F, secondary press filtration: become qualifying liquid through the secondary press filtration again;
G, electrolysis: electrolysing period is 24 hours, groove temperature 40-46 degree, pH value is between 6.8-7.4;
H, go out the groove passivation, rinses product to without sulphur-cake, then dry, peel off and get final product.
2. production method according to claim 1, it is characterized in that: in step B, in anolyte, the content concn of Mn is 13g/l, and the H content concn is 40g/l; Then under the temperature environment of 48 ℃, react 18 minutes; Add the sulfuric acid that is equivalent to breeze weight 40%, the concentration of sulfuric acid is 96% again, Leaching reaction 5 hours, and spent acid concentration is controlled at 1.0g/L-1.1g/L.
3. production method according to claim 1, is characterized in that: in steps A, adopt Vertical Mill negative pressure powder-making machine to carry out powder process.
4. production method according to claim 1 is characterized in that: in step e and step F, described filtering equipment adopts high pressure eardrum pressure filter.
5. production method according to claim 1, it is characterized in that: in step G, the electrolyzer that adopts is made by the RPP material.
6. production method according to claim 1, is characterized in that: in step H, adopt ultrasonic wave to wash plate and washed plate.
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| CN201310344630.6A CN103451673B (en) | 2013-08-08 | 2013-08-08 | The production method of electrolytic metal Mn |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104018184A (en) * | 2014-06-25 | 2014-09-03 | 张安良 | Brand new method of producing electrolytic manganese metal |
| CN107858702A (en) * | 2017-12-01 | 2018-03-30 | 大新县科学技术情报研究所 | A kind of production method of electrolytic manganese metal |
| CN109208031A (en) * | 2018-11-19 | 2019-01-15 | 四川中哲新材料科技有限公司 | A kind of production method of electrolytic manganese metal |
| CN110551898A (en) * | 2019-09-16 | 2019-12-10 | 中信大锰矿业有限责任公司 | treatment method of electrolytic manganese slag |
| CN110732543A (en) * | 2018-10-18 | 2020-01-31 | 庞炼红 | Method for jointly producing cement clinker and ammonia water by electrolyzing metal manganese waste residue and gypsum |
| CN114108030A (en) * | 2021-11-29 | 2022-03-01 | 靖西市锰矿有限责任公司 | Method for producing electrolytic manganese metal |
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| CA402636A (en) * | 1942-02-03 | Henry Hannay William | Electrolytic manganese processing | |
| CN102094124A (en) * | 2011-03-10 | 2011-06-15 | 中信锦州金属股份有限公司 | Method for producing electrolytic metal manganese and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104018184A (en) * | 2014-06-25 | 2014-09-03 | 张安良 | Brand new method of producing electrolytic manganese metal |
| CN107858702A (en) * | 2017-12-01 | 2018-03-30 | 大新县科学技术情报研究所 | A kind of production method of electrolytic manganese metal |
| CN110732543A (en) * | 2018-10-18 | 2020-01-31 | 庞炼红 | Method for jointly producing cement clinker and ammonia water by electrolyzing metal manganese waste residue and gypsum |
| CN109208031A (en) * | 2018-11-19 | 2019-01-15 | 四川中哲新材料科技有限公司 | A kind of production method of electrolytic manganese metal |
| CN110551898A (en) * | 2019-09-16 | 2019-12-10 | 中信大锰矿业有限责任公司 | treatment method of electrolytic manganese slag |
| CN114108030A (en) * | 2021-11-29 | 2022-03-01 | 靖西市锰矿有限责任公司 | Method for producing electrolytic manganese metal |
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