CN102491423A - Method for preparing manganese sulfate from sulfur-containing slag - Google Patents
Method for preparing manganese sulfate from sulfur-containing slag Download PDFInfo
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- CN102491423A CN102491423A CN2011104009656A CN201110400965A CN102491423A CN 102491423 A CN102491423 A CN 102491423A CN 2011104009656 A CN2011104009656 A CN 2011104009656A CN 201110400965 A CN201110400965 A CN 201110400965A CN 102491423 A CN102491423 A CN 102491423A
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- acid leaching
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Abstract
The invention relates to a method for preparing manganese sulfate from sulfur-containing slag. The method comprises the following steps of: calcining acid leaching electrolytic manganese residues and lead-zinc tailings or limestone at a high temperature, calcining stone coal-extracted vanadium acid leaching residues and lead-zinc tailings or limestone at a high temperature, or calcining acid leaching electrolytic manganese residues, stone coal-extracted vanadium acid leaching residues, lead-zinc tailings and limestone together at a high temperature, calcining coal-extracted vanadium acid leaching residues and acid leaching electrolytic manganese residues to obtain cement clinker or a cement mixture, compressing a mixed gas of sulfur dioxide and sulfur trioxide produced by calcining, introducing into mixed slurry consisting of pyrolusite, manganese spar and water in the liquid-solid ratio of 3:1-8:1, and leaching while continually stirring for 4-10 hours; filtering and removing impurities to obtain a manganese sulfate solution; and evaporating the solution, concentrating, crystalizing and drying to obtain finished manganese sulfate.
Description
Technical field
The present invention relates to the method that a kind of sulfur-bearing slag prepares manganous sulfate
Background technology
The acidleach electrolytic manganese residues is with slag remaining behind the sulfuric acid to leach rhodochrosite, and wherein sulfate radical content is more than 20%, produces about 9 tons of the acidleach electrolytic manganese residues of 1 ton of electrolytic manganese generation.The extracting vanadium from stone coal acid leaching residue is with the slag under the surplus acidleach electrolytic manganese residues behind the sulfuric acid to leach bone coal, wherein also contains a large amount of sulfate radicals, produces 1 ton of V
2O
5About 150 tons of the slag that produces.Pb-Zn tailings is that plumbous zinc ore factory adopts the powdery or the fine sand shape slag of discharging after the flotation process ore dressing, produces about 60 tons of the Pb-Zn tailings slag of 1 ton of lead and zinc concentrate generation.These three kinds of scoriaceous quantity dischargeds are very big, caused serious environmental to pollute and potential safety hazard.
Because sulfate radical content is higher in acidleach electrolytic manganese residues and the extracting vanadium from stone coal acid leaching residue, fully utilize comparatively difficulty under normal conditions, cost is high.Directly calcining can change it into, to remove sulfate radical wherein, does not have cost advantage but mixed gas is continued to be converted into sulfuric acid.
Dioxide-containing silica is very high in this area acidleach electrolytic manganese residues and the extracting vanadium from stone coal acid leaching residue, and the mass percent beyond the sulfate radical has reached more than 60%, and these two kinds of slags can obtain cement mixture after high-temperature calcination; Calcium carbonate content in the local plumbous zinc ore slag is high, reached about 86%, this slag respectively with above-mentioned two kinds of slags, perhaps simultaneously after high-temperature calcination, can obtain cement clinker with above-mentioned two kinds of slags.Sulfurous gas that calcining produces and sulphur trioxide mixed gas through removal of impurities, obtain to can be used for producing the manganous sulfate electrolytic solution of electrolytic manganese after using the mixed ore pulp of pyrolusite and rhodochrosite to absorb, and perhaps crystallizing and drying is produced the manganous sulfate solid.
Summary of the invention
The purpose of this invention is to provide the method that a kind of cost is low, the effective sulfur-bearing slag of comprehensive utilization prepares manganous sulfate.
The present invention calcines acidleach electrolytic manganese residues, extracting vanadium from stone coal acid leaching residue respectively to obtain cement mixture; Perhaps acidleach electrolytic manganese residues or extracting vanadium from stone coal acid leaching residue are mixed high-temperature calcination with plumbous zinc tailings or Wingdale etc.; Obtain cement clinker; And, obtain manganous sulfate through steps such as removal of impurities again with the mixed serum absorption that the sulfurous gas and the sulphur trioxide mixed gas of above two kinds of calcining manners generation are formed with pyrolusite, rhodochrosite and water, realize the complete recycle of slag composition.
The sulfur-bearing slag is calcined by following dual mode:
1, with acidleach electrolytic manganese residues or extracting vanadium from stone coal acid leaching residue and plumbous zinc tailings or Wingdale by 1: the mixed of 3.5-4.5; Be equipped with a spot of diaspore or bauxitic clay and iron powder; Make the outer various oxide mass per-cents of sulphur removal in the mixture be: CaO 42.5-44.6%, SiO
213.3-14.5%, Al
2O
33-4.5%, Fe
2O
3After 1.3-3%, mixture are ground to 180 orders, obtain cement clinker 1320 ℃ of-1460 ℃ of calcinings;
2, acidleach electrolytic manganese residues or extracting vanadium from stone coal acid leaching residue are pressed arbitrary proportion mixed grinding to 120 order after, obtain cement mixture 1150 ℃ of-1200 ℃ of calcinings;
The sulfurous gas that above two kinds of calcining manners are produced and sulphur trioxide mixed gas feed the mixed serum of pyrolusite, rhodochrosite and water composition, obtain manganous sulfate through steps such as removal of impurities, concentrated, crystallizations again.The liquid-solid ratio of the mixed serum that pyrolusite, rhodochrosite and water are formed is 3: 1-8: 1; Wherein in the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, in the mixed serum quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.
Adopt method of the present invention to prepare manganous sulfate; Realized the recycle of sulfate radical in acidleach electrolytic manganese residues, the extracting vanadium from stone coal acid leaching residue; Reduced the production cost that pickling process prepares manganous sulfate, and owing to be that slightly acidic condition leaches, impurity such as calcium magnalium iron is less relatively in the leach liquor; The manganous sulfate purity that obtains is high, remarkable in economical benefits.
Mass consumption slag of the present invention has solved a large amount of environmental pollution and the potential safety hazards that cause of stacking of extracting vanadium from stone coal acid leaching residue, acidleach electrolytic manganese residues and Pb-Zn tailings, and environmental benefit is outstanding.
Embodiment:
Embodiment 1
The acidleach electrolytic manganese residues is mixed with the mass ratio of Pb-Zn tailings by 1: 3.5, be equipped with a spot of diaspore and iron powder, make the quality mass percent of the various oxide compounds outside the sulphur removal in the mixture be: CaO 43.4%, SiO
213.6%, Al
2O
33.8%, Fe
2O
32.7%, mixture is ground to 180 orders after, obtain cement clinker 1320 ℃ of-1440 ℃ of calcinings.Mixed serum with the sulfurous gas that produces and sulphur trioxide mixed gas feeding pyrolusite and rhodochrosite after drying and compression.Pyrolusite and rhodochrosite mixed serum are prepared as follows: pyrolusite and rhodochrosite mixing raw material are ground to 100 orders; Adding water then, to stir into liquid-solid ratio be 4: 1 ore pulp; In the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, the quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.Sulfurous gas and sulphur trioxide mixed gas are pressed into from the agitation vat bottom, and Mass becomes even small bubbles to get into ore pulp through the stainless steel sieve plate, and ore pulp is under the cat head spray, and whole process constantly stirs, and extraction time is 6 hours, and extraction temperature is 80 ℃.Through filtering, add ammoniacal liquor and be neutralized to pH～7 hydrolysis deironing after leaching liquid flows out from the absorption tower, add the Sodium Dimethyldithiocarbamate removing heavy metals again, obtain qualified manganese sulfate solution electrolysis after the smart filter and use.
Embodiment 2
The extracting vanadium from stone coal acid leaching residue is mixed with the mass ratio of Pb-Zn tailings by 1: 4, be equipped with a spot of bauxitic clay and iron powder, make the outer various oxide mass per-cents of sulphur removal in the mixture be: CaO42.5%, SiO
214.5%, Al
2O
33.1%, Fe
2O
31.9%, mixture is ground to 180 orders after, obtain cement clinker 1330 ℃ of-1450 ℃ of calcinings.Sulfurous gas and sulphur trioxide mixed gas drying that calcining produces are also compressed the mixed serum that the back feeds pyrolusite and rhodochrosite.The mixed serum of pyrolusite and rhodochrosite is prepared as follows: pyrolusite and rhodochrosite mixing raw material are ground to 100 orders; Adding water, to stir into liquid-solid ratio be 5: 1 ore pulp; In the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, the quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.The mixed gas of sulfurous gas and sulphur trioxide is pressed into from the agitation vat bottom, and Mass becomes even small bubbles to get into ore pulp through the stainless steel sieve plate, and ore pulp is under the cat head spray, and whole process adopts compartment to stir, and extraction time is 7 hours, and extraction temperature is 70 ℃.Leaching liquid flows out after-filtration from the absorption tower, adds milk of lime and transfers pH=6～7 deironing, refilters an amount of barium sulphide removing heavy metals of back adding, obtains manganese sulfate solution after the filtration, the evaporation concentration manganese sulfate solution, and crystallization, drying obtain the product manganous sulfate.
Embodiment 3
The acidleach electrolytic manganese residues is mixed with the mass ratio of Wingdale by 1: 4.5, be equipped with a spot of diaspore and iron powder, make the outer various oxide mass per-cents of sulphur removal in the mixture be: CaO42.9%, SiO
213.9%, Al
2O
33.6%, Fe
2O
32.1%, mixture is ground to 180 orders after, obtain cement clinker 1360 ℃ of-1460 ℃ of calcinings.With calcining with the sulfurous gas that produces and sulphur trioxide mixed gas through the vitriol oil dry and with the air mixed compression after the mixed serum of feeding pyrolusite and rhodochrosite.Pyrolusite and rhodochrosite mixed serum are prepared as follows: pyrolusite and rhodochrosite mixing raw material are ground to 100 orders; Adding water, to stir into liquid-solid ratio be 4: 1 ore pulp; In the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, the quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.Sulfurous gas and sulphur trioxide mixed gas are pressed into from the agitation vat bottom, and Mass becomes even small bubbles to get into ore pulp through the stainless steel sieve plate, and ore pulp is under the cat head spray, and whole process adopts compartment to stir, and extraction time is 8 hours, and extraction temperature is 80 ℃.Leaching liquid flows out after-filtration from the absorption tower, adds milk of lime and transfers pH=6～7 deironing, refilters an amount of barium sulphide removing heavy metals of back adding, obtains manganese sulfate solution after the filtration, the evaporation concentration manganese sulfate solution, and crystallization, drying obtain the product manganous sulfate.
Embodiment 4
The extracting vanadium from stone coal acid leaching residue is mixed with the mass ratio of Wingdale by 1: 4.3, be equipped with a spot of diaspore and iron powder, make the outer various oxide mass per-cents of sulphur removal in the mixture be: CaO 42.6%, SiO
214.1%, Al
2O
33%, Fe
2O
31.35%, mixture is ground to 180 orders after, obtain cement clinker 1360 ℃ of-1460 ℃ of calcinings.With calcining with the sulfurous gas that produces and sulphur trioxide mixed gas through the vitriol oil dry and with the air mixed compression after the mixed serum of feeding pyrolusite and rhodochrosite.Pyrolusite and rhodochrosite mixed serum are prepared as follows: pyrolusite and rhodochrosite mixing raw material are ground to 100 orders; Adding water, to stir into liquid-solid ratio be 4: 1 ore pulp; In the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, the quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.Sulfurous gas and sulphur trioxide mixed gas are pressed into from the agitation vat bottom, and Mass becomes even small bubbles to get into ore pulp through the stainless steel sieve plate, and ore pulp is under the cat head spray, and whole process adopts compartment to stir, and extraction time is 8 hours, and extraction temperature is 80 ℃.Leaching liquid flows out after-filtration from the absorption tower, adds milk of lime and transfers pH=6～7 deironing, refilters an amount of barium sulphide removing heavy metals of back adding, obtains manganese sulfate solution after the filtration, the evaporation concentration manganese sulfate solution, and crystallization, drying obtain the product manganous sulfate.
Embodiment 5
Extracting vanadium from stone coal acid leaching residue, acidleach electrolytic manganese residues are mixed with the mass ratio of Pb-Zn tailings by 0.5: 0.5: 3.8, be equipped with a spot of diaspore and iron powder, make the outer various oxide mass per-cents of sulphur removal in the mixture be: CaO 43.3%, SiO
213.7%, Al
2O
34.5%, Fe
2O
32.3%, mixture is ground to 180 orders after, obtain cement clinker 1340 ℃ of-1440 ℃ of calcinings.With calcining with the sulfurous gas that produces and sulphur trioxide mixed gas through the vitriol oil dry and with the air mixed compression after the mixed serum of feeding pyrolusite and rhodochrosite.Pyrolusite and rhodochrosite mixed serum are prepared as follows: pyrolusite and rhodochrosite mixing raw material are ground to 100 orders; Adding water, to stir into liquid-solid ratio be 5: 1 ore pulp; In the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, the quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.Sulfurous gas and sulphur trioxide mixed gas are pressed into from the agitation vat bottom, and Mass becomes even small bubbles to get into ore pulp through the stainless steel sieve plate, and ore pulp is under the cat head spray, and whole process adopts compartment to stir, and extraction time is 10 hours, and extraction temperature is 80 ℃.Leaching liquid flows out after-filtration from the absorption tower, adds milk of lime and transfers pH=6～7 deironing, refilters an amount of barium sulphide removing heavy metals of back adding, obtains manganese sulfate solution after the filtration, the evaporation concentration manganese sulfate solution, and crystallization, drying obtain the product manganous sulfate.
Embodiment 6
Extracting vanadium from stone coal acid leaching residue, acidleach electrolytic manganese residues are mixed by 0.2: 0.8: 4 mass ratio with Wingdale, be equipped with a spot of diaspore and iron powder, make the mass percent of the outer various oxide compounds of sulphur removal in the mixture be: CaO 43.3%, SiO
213.5%, Al
2O
34%, Fe
2O
32.6%, be ground to 180 orders after, obtain cement clinker 1340 ℃ of-1440 ℃ of calcinings.With calcining with the sulfurous gas that produces and sulphur trioxide mixed gas through the vitriol oil dry and with the air mixed compression after the mixed serum of feeding pyrolusite and rhodochrosite.Pyrolusite and rhodochrosite mixed serum are prepared as follows: pyrolusite and rhodochrosite mixing raw material are ground to 100 orders; Adding water, to stir into liquid-solid ratio be 3: 1 ore pulp; In the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, the quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.Sulfurous gas and sulphur trioxide mixed gas are pressed into from the agitation vat bottom, and Mass becomes even small bubbles to get into ore pulp through the stainless steel sieve plate, and ore pulp is under the cat head spray, and whole process adopts compartment to stir, and extraction time is 7 hours, and extraction temperature is 80 ℃.Leaching liquid flows out after-filtration from the absorption tower, adds milk of lime and transfers pH=6～7 deironing, refilters an amount of barium sulphide removing heavy metals of back adding, obtains manganese sulfate solution after the filtration, the evaporation concentration manganese sulfate solution, and crystallization, drying obtain the product manganous sulfate.
Embodiment 7
The extracting vanadium from stone coal acid leaching residue is mixed with arbitrary proportion with the acidleach electrolytic manganese residues, obtain cement mixture 1250 ℃ of calcinings.Calcining is fed sulfurous gas that produces and sulphur trioxide mixed gas compression back the mixed serum of pyrolusite and rhodochrosite.Pyrolusite and rhodochrosite mixed serum are prepared as follows: pyrolusite and rhodochrosite mixing raw material are ground to 100 orders; Adding water, to stir into liquid-solid ratio be 8: 1 ore pulp; In the mixed serum quality of pyrolusite be in itself and the mixed gas the theoretical reacting weight of sulfurous gas 92%, the quality of rhodochrosite be in itself and the mixed gas sulphur trioxide theory reacting weight 95%.Sulfurous gas and sulphur trioxide mixed gas are pressed into from the agitation vat bottom, and Mass becomes even small bubbles to get into ore pulp through the stainless steel sieve plate, and ore pulp is under the cat head spray, and whole process adopts compartment to stir, and extraction time is 8 hours, and extraction temperature is 80 ℃.Leaching liquid flows out after-filtration from the absorption tower, adds milk of lime and transfers pH=6～7 deironing, refilters an amount of barium sulphide removing heavy metals of back adding, obtains manganese sulfate solution after the filtration, the evaporation concentration manganese sulfate solution, and crystallization, drying obtain the product manganous sulfate.
Claims (1)
1. a sulfur-bearing slag prepares the method for manganous sulfate; It is characterized in that acidleach electrolytic manganese residues or extracting vanadium from stone coal acid leaching residue and plumbous zinc tailings or Wingdale by 1: the mass percent of 3.5-4.5 is mixed; Be equipped with a spot of diaspore or bauxitic clay and iron powder; Make beyond the sulphur removal that various oxide mass per-cents are in the raw ingredients: CaO 42.5-44.6%, SiO
213.3-14.5%, Al
2O
33-4.5%, Fe
2O
31.3-3%, the mixture raw material are ground to 180 orders after, obtain cement clinker 1320 ℃ of-1460 ℃ of calcinings; Or after acidleach electrolytic manganese residues or extracting vanadium from stone coal acid leaching residue pressed arbitrary proportion mixed grinding to 120 order, obtain cement mixture 1150 ℃ of-1300 ℃ of calcinings; Sulfurous gas and sulphur trioxide mixed gas that above two kinds of calcining manners produce are pressed liquid-solid mass ratio 3: 1-8 with pyrolusite, rhodochrosite and water: the mixed serum of 1 composition absorbs, and obtains manganous sulfate through filtration, removal of impurities, condensing crystal again.
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| CN103014760A (en) * | 2013-01-09 | 2013-04-03 | 广西有色金属集团汇元锰业有限公司 | Production method of electrolytic manganese metal |
| CN106048651A (en) * | 2016-08-03 | 2016-10-26 | 宁夏天元锰业有限公司 | Electrolytic manganese metal production method |
| CN108483501A (en) * | 2018-07-04 | 2018-09-04 | 绵阳师范学院 | A kind of method of comprehensive utilization of electrolytic manganese residues water lotion |
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| CN108483501A (en) * | 2018-07-04 | 2018-09-04 | 绵阳师范学院 | A kind of method of comprehensive utilization of electrolytic manganese residues water lotion |
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