CN103114303A - Process method for deep purification in production for high-purity non-selenium electrolytic manganese metal and additive - Google Patents
Process method for deep purification in production for high-purity non-selenium electrolytic manganese metal and additive Download PDFInfo
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- CN103114303A CN103114303A CN2013100742825A CN201310074282A CN103114303A CN 103114303 A CN103114303 A CN 103114303A CN 2013100742825 A CN2013100742825 A CN 2013100742825A CN 201310074282 A CN201310074282 A CN 201310074282A CN 103114303 A CN103114303 A CN 103114303A
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Abstract
The invention provides a process method for producing electrolytic manganese metal by using ammonium sulphite as an antioxidant for replacing SeO2, and an additive. In a production process, the methods of deep purification, triple press filtration, and layered filtration for the upper-layer clear solution and the lower-layer turbid solution of the purified solution are adopted; during composition in deep purification, the residual heavy-metal and non-metallic impurities in solution are removed by adopting aluminium sulphate, an additive I, active carbon, and the methods of gravity settling and adsorption, and an additive II is added in electrolytic new solution (qualified solution) to improve the electrolytic performance of the solution. Therefore, compared with the traditional production process for electrolytic manganese metal by using SeO2 as an antioxidant or using SO2 as an antioxidant, purification effect (purity) for the electrolytic new solution (qualified solution) is improved, current efficiency is increased, power consumption is reduced, and the purposes of improving product quality, saving energy and reducing consumption, and protecting environment are achieved. The method is a new process method worth of popularization and use.
Description
Technical field
The present invention relates to the electrolytic metal Mn technical field, particularly relate to a kind of without selenium electrolytic metal Mn advanced purification process method and additive technology.
Background technology
From the electrolytic manganese industrial development, oxidation inhibitor (additive) plays a part particularly important in whole electrolytic manganese industry, and middle forties is just found the oxidation inhibitor that comparatively is fit to electrolytic manganese, mainly is SeO
2And SO
2In the actual production, use SeO
2As oxidation inhibitor, from current efficiency, stable aspect is better than SO
2, but SeO
2Market value is higher, or highly toxic substance, and human body is had larger injury, also pollute the environment simultaneously, and selenium enters in the product, has reduced quality product, has limited the Application Areas of manganese.
CN102703926A " without selenium electrolytic metal Mn High-efficient Production additive " adopts thiosulphate, polythionate and lays particular stress on a kind of in the sulphite or oxidation inhibitor that their combination forms, has substituted the existing SeO of using
2Make oxidation inhibitor and be used for electrolytic manganese production.This technology has solved replacement SeO
2Make the problem of oxidation inhibitor, but the additive problem that does not have to solve the defective workmanship in the existing electrolytic metal Mn production and improve the electrolysis performance.
Tradition SeO
2Make the antioxidant processing method, leaching, oxidation, neutralization, sulfuration be integrated in the leaching barrel carry out, the secondary-cleaned operation is not set, will not leave standstill the supernatant liquid after the purification, the muddy liquid of lower floor carries out respectively filtration treatment, solution is produced in the process solution is generally only carried out secondary filtration, and sulfuration removing heavy-metal impurities operation generally only adopts the SDD(Sodium Dimethyldithiocarbamate) a kind of, the beavy metal impurity content such as Cu, Ni and Co zinc is generally higher in the solution; Adopt tin anhydride to make oxidation inhibitor, in the cleaning section the general time shorter, solution can't carry out subsiding and purifying.CN102296323A " method for producing electrolytic manganese metal by two-ore manufacturing system ", affiliated system is by liquid processed unit, sulfuration removal of impurity unit, clean unit and electrolysis cells form, though will leach in this invention, oxidation, neutralization, sulfuration is divided into two unit and carries out, after solution carried out secondary filtration, also used the strong oxidizer hydrogen peroxide to purify again, leaving standstill operation has selected Tai-Ace S 150 to make flocculation agent, but this invention is still adopted selenium to make oxidation inhibitor and is produced electrolytic metal Mn, fail to overcome the drawback that selenium brings as oxidation inhibitor, and not yet really find high-efficiency purification process method and deep purifying and improve the additive of electrolysis performance.
Summary of the invention
The purpose of this invention is to provide a kind of SeO that do not adopt
2Make oxidation inhibitor, can overcome SeO
2Production cost is high, severe toxicity, contaminate environment and human body damaged, and selenium is residual on the quality product impact, can overcome again the deficiency in traditional Process of Electrolytic Manganese.Particularly adopt the processing method of deep purifying, three press filtrations, the muddy liquid layered filtration of scavenging solution supernatant liquid and lower floor; Combined Mining is removed the impurity such as heavy metal residual in the solution is nonmetal with the method for Tai-Ace S 150, No. 1 additive, gac, gravity settling and absorption in the deep purifying, adds No. 2 additives in the new liquid of electrolysis (qualifying liquid) and improves electrolysis of solutions performance.
According to its processing method of purpose of the present invention be:
Selected technical recipe additive and design parameter thereof:
1. SDD(Sodium Dimethyldithiocarbamate), two kinds of removing heavy-metal impurities scavenging agents of ammonium sulfide consumption is pressed the beavy metal impurity percentage composition such as Cu, Ni and Co zinc and is added Song Taoxian ore deposit, general every cubic metre of solution 150～200g(Guizhou).
2. 1 kilogram of every cubic metre of qualifying liquid of ammonium sulphite addition (contains sulfurous gas 0.4～0.5g/L).
3. Tai-Ace S 150 is mixed with 20% aqueous solution, by 10 liters of interpolations of every cubic metre of solution.
4. No. 1 additive is anionic, and the polyacrylamide of molecular weight about 1,000 ten thousand is mixed with the 1g/L aqueous solution, adds by 2～2.5 liters of additions of every cubic metre of qualifying liquid.
5. gac adds by every cubic metre of qualifying liquid 50g addition.
6. No. 2 additives are non-ionic type, and molecular weight is about 8,000,000 polyacrylamide
Be mixed with the 1g/L aqueous solution, add by 2～2.5 liters of additions of every cubic metre of qualifying liquid.
Manganese carbonate ore is ground into negative 100 orders (90 ﹪ sieve), when final volume is soaked in pump anolyte to 1/4～1/3 first, termination of pumping, open to leach and stir, drop into 100 order manganous carbonate breezes, put sulfuric acid and stir leaching in 1～2 hour, reach more than 93% in leaching yield, when soaking whole pH value to 3.5～4.5(spent acid 0.5～1.5g/L), add the dioxide ore for manganese stone flour and carry out oxidation, stirred 0.5 hour, after the sampling detection is qualified, add ammoniacal liquor and carry out neutralization reaction, in and pH value to 6.5～6.6, then carry out press filtration first time, the clear liquid of coarse filtration is this time imported sulfuration barrel, muddy liquid imports leaching barrel or the coarse filtration pump is inhaled the pond, and filter residue is stacked.Filtrate adds the SDD(Sodium Dimethyldithiocarbamate), two kinds of removing heavy-metal impurities scavenging agents of ammonium sulfide, stirs and finished sulfuration and primary purification technique in 0.5～1 hour, carry out the secondary press filtration after the detection of taking a sample is qualified, two pressure solution liquid import purification barrel, evenly add simultaneously aluminum sulfate aqueous solution, stirred 0.5～1 hour, put into ammoniacal liquor and regulate pH value to 6.5～6.6, add activated carbon, stirred 0.5～1 hour, and added No. 1 additive, heavy clear 30～48 hours of secondary-cleaned, after reaching the secondary-cleaned requirement, enter three pressure-sizing filter.Open the upper strata tap valve, the clear liquid pipe is moved into muddy liquid pump inhale the pond, enter muddy hydraulic pressure filter and carry out press filtration, until the upper strata liquid discharging tube emit solution limpid after, again liquid discharging tube is moved into clear liquid pump and inhale the pond, after supernatant liquid discharges, open lower floor's tap valve, emit after muddy liquid enters muddy hydraulic pressure filter and carry out press filtration, solution enters purification barrel and again purifies.The clear liquid that the clear liquid pressure filter is press-filtered out imports turnover barrel or header tank, in importing process, adds ammonium sulphite and No. 2 additives and is the new liquid of electrolysis (qualifying liquid).
During new fluting, qualified additional liquid requirement is: Mn
2+34g/L, (NH
4)
2SO
4130g/L, SO
20.5g/L, No. 2 additive 2.0mg/L, PH6.6
Put into the empty negative plate that flooded sodium silicate solution, pass into direct supply and carry out electrolysis, bath voltage 4.2～5.0V, electrolysing period 24 h～36h, tank liquor (negative electrode) Mn
2+12～14g/L, tank liquor pH value 7.5～8.0,34～37 ℃ of groove temperature.The product that electrolysis is good carries out aftertreatment, behind the purifying products, washing, dry, peel off, classification, metering, packing, warehouse-in.
The present invention and traditional SeO
2Making the electrolytic metal Mn production technique of antioxidant and compare, mainly is to have adopted following technique:
1. will vulcanize, primary purification arranges separately operation and carries out except metallic impurity;
2. deep purifying: arrange and leave standstill the secondary-cleaned operation, and will leave standstill that solution behind the secondary-cleaned carries out supernatant liquid, the muddy liquid of lower floor carries out respectively filtration treatment, the muddy liquid of the lower floor after the filtration again purifies, filters;
3. solution is produced in the process solution is carried out three filtrations;
4. sulfuration, the primary purification removing heavy-metal impurities adopts the SDD(Sodium Dimethyldithiocarbamate), two kinds of removing heavy-metal impurities scavenging agents of ammonium sulfide are used, and reach the beavy metal impurities such as better removal Cu, Ni and Co zinc;
5. adopt and press ammonium sulfate generation sulfurous gas to make oxidation inhibitor replacement tin anhydride;
6. leave standstill and adopt Tai-Ace S 150, No. 1 additive, activated carbon to be used and to make precipitation agent, sorbent material in the secondary-cleaned operation, utilize gravity settling, adsorption method to purify and remove plurality of impurities;
7. add No. 2 additives in the qualifying liquid (new liquid) and improve qualifying liquid electrolysis performance;
Just because of the novel process of above uniqueness has been arranged; not only overcome with selenium and made the drawback that antioxidant brings; solve again traditional technology method removing heavy metals and thoroughly particularly can't not remove the nonmetal problem of bringing; and the traditional technology that the present invention and former employing sulfurous gas are done oxidation inhibitor production has relatively improved current efficiency 6～10%; consumption of direct current reduces by 500～700KWh/T; improve quality product, reduced cost, protected environment.
Description of drawings
Fig. 1 is technological process block-diagram of the present invention.
Embodiment
Now by reference to the accompanying drawings technical process of the present invention is further described:
Take the Song Taoxian of Guizhou Province manganese carbonate ore as example, contain bivalent manganese 16%, produce one ton of high-purity selenium-free manganese metal, take anolyte as production basis, anolyte contains manganese 14g/L, (NH
4)
2SO
4120g/L, sulfuric acid 35g/L, metal total yield 80% consumes qualified solution 50M
3Be the embodiment foundation.
1. the carbonic acid ore powder is broken into negative 100 orders (90 ﹪ sieve), adding first anolyte to 1/4～1/3 when soaking end-body, termination of pumping, open to leach and stir, add 7.8 tons of 100 purpose manganous carbonate breezes, put 2.93 tons in sulfuric acid and stir leaching in 1～2 hour, reach more than 93% in leaching yield, add Manganse Dioxide breeze 300Kg when soaking whole pH value to 3.5～4.5(spent acid 0.5～1.5g/L) and carry out oxidation, stirred 0.5 hour, add the ammoniacal liquor neutralization, be neutralized to PH6.5～6.6, carry out a press filtration, with the clear liquid importing sulfuration bucket of coarse filtration, muddy liquid imports leaching barrel or coarse filtration pump cuvette, and filter residue is stacked.Filtrate adds the SDD(Sodium Dimethyldithiocarbamate) 10～14Kg, 3～5 liters of ammonium sulfide solutions stirred 0.5～1.0 hour, after the sampling detection is qualified, carried out the secondary press filtration.Two pressure solution liquid import purification barrel, evenly add simultaneously aluminum sulfate aqueous solution 0.5M
3,, stirred 0.5～1 hour, put into ammoniacal liquor and regulate pH value to 6.5～6.6, add activated carbon 2500g, stirred 0.5 hour, add 125 liters of stirrings of No. 1 additive aqueous solution 25 minutes, make its natural subsidence, heavy after clear 30～48 hours, carry out three press filtrations.Open the upper strata tap valve, the clear liquid pipe is moved into muddy liquid pump inhale the pond, enter muddy hydraulic pressure filter and carry out press filtration, until the upper strata liquid discharging tube emit solution limpid after, again liquid discharging tube is moved into clear liquid pump and inhale the pond, after supernatant liquid discharges, open lower floor's tap valve, emit muddy liquid and enter muddy hydraulic pressure filter and carry out after the press filtration solution and enter purification barrel and again purify.The clear liquid that the clear liquid pressure filter is press-filtered out imports turnover barrel or header tank, in importing process, adds 125 liters of ammonium sulphite 25 kilograms (being mixed with the aqueous solution) and No. 2 additive aqueous solution, is the new liquid of electrolysis (qualifying liquid).
The qualifying liquid gravity flow enters in the electrolyzer that has assembled.During new fluting, new liquid requires: Mn
2+34g/L, (NH
4)
2SO
4130g/L, SO
20.5g/L, No. 2 additive 2.0mg/L PH6.6
Put into the empty negative plate that flooded sodium silicate solution, pass into direct supply and carry out electrolysis, bath voltage 4.2～5.0V, electrolysing period 24 h～36h, tank liquor (negative electrode) Mn
2+12～14g/L, tank liquor pH value 7.5～8.0,32～35 ℃ of groove temperature.The product that electrolysis is good carries out aftertreatment, behind the purifying products, washing, dry, peel off, classification, metering, packing, warehouse-in.
Claims (2)
1. High pure no-Se electrolyzed metal Mn is produced advanced purification process method and additive, it is characterized in that: manganese carbonate ore is ground into negative 100 orders (90 ﹪ sieve), when final volume is soaked in pump anolyte to 1/4～1/3 first, termination of pumping, open to leach and stir, drop into 100 order manganous carbonate breezes, put sulfuric acid and stir leaching in 1～2 hour, reach more than 93% in leaching yield, when soaking whole pH value to 3.5～4.5(spent acid 0.5～1.5g/L), add the dioxide ore for manganese stone flour and carry out oxidation, stirred 0.5 hour, after the sampling detection is qualified, add ammoniacal liquor and carry out neutralization reaction, in and pH value to 6.5～6.6, then carry out the press filtration first time, bucket is vulcanized in this time clear liquid importing of coarse filtration, muddy liquid imports leaching barrel or the coarse filtration pump is inhaled the pond, filter residue is stacked, filtrate adds the SDD(Sodium Dimethyldithiocarbamate), two kinds of removing heavy-metal impurities scavenging agents of ammonium sulfide, stir and finished sulfuration and primary purification technique in 0.5～1 hour, carry out the secondary press filtration after the sampling detection is qualified, two pressure solution liquid import purification barrel, evenly add simultaneously aluminum sulfate aqueous solution, stirred 0.5～1 hour, put into ammoniacal liquor and regulate pH value to 6.5～6.6, add activated carbon, stirred 0.5～1 hour, add No. 1 additive, heavy clear 30～48 hours of secondary-cleaned, reach the secondary-cleaned requirement after, enter three pressure-sizing filter, open the upper strata tap valve, the clear liquid pipe is moved into muddy liquid pump inhales the pond, enter muddy hydraulic pressure filter and carry out press filtration, until the upper strata liquid discharging tube emit solution limpid after, again liquid discharging tube is moved into clear liquid pump and inhale the pond, after supernatant liquid discharges, open lower floor's tap valve, emit after muddy liquid enters muddy hydraulic pressure filter and carry out press filtration, solution enters purification barrel and again purifies, the clear liquid that the clear liquid pressure filter is press-filtered out imports turnover barrel or header tank, in importing process, adds ammonium sulphite and No. 2 additives and is the new liquid of electrolysis (qualifying liquid), during new fluting, qualified additional liquid requirement is: Mn
2+34g/L, (NH
4)
2SO
4130g/L, SO
20.5g/L, No. 2 additive 2.0mg/L, PH6.6
Put into the empty negative plate that flooded sodium silicate solution, pass into direct supply and carry out electrolysis, bath voltage 4.2～5.0V, electrolysing period 24 h～36h, tank liquor (negative electrode) Mn
2+12～14g/L, tank liquor pH value 7.5～8.0,34～37 ℃ of groove temperature, the product that electrolysis is good carries out aftertreatment, behind the purifying products, washing, dry, peel off, classification, metering, packing, warehouse-in.
2. High pure no-Se electrolyzed metal Mn according to claim 1 is produced advanced purification process method and additive, it is characterized in that: the manganese dioxide powder that adds is to drop into by 10～15% of manganese carbonate ore weight.
3. High pure no-Se electrolyzed metal Mn according to claim 1 is produced advanced purification process method and additive, the SDD(Sodium Dimethyldithiocarbamate that sulfuration, primary purification add), two kinds of removing heavy-metal impurities scavenging agents of ammonium sulfide it is characterized in that:, consumption is that general every cubic metre of solution adds 150～200g(Guizhou Song Taokuang by beavy metal impurity percentage compositions such as Cu, Ni and Co zinc).
4. High pure no-Se electrolyzed metal Mn according to claim 1 is produced advanced purification process method and additive, it is characterized in that: Tai-Ace S 150 is mixed with the 20 % aqueous solution, add 10 liters by every cubic metre, No. 1 additive is the polyacrylamide of Anion molecule amount about 1,000 ten thousand, be mixed with the 1g/L aqueous solution, by 2～2.5 liters of interpolations of every cubic metre of qualifying liquid, gac adds by every cubic metre of 50g.
5. High pure no-Se electrolyzed metal Mn according to claim 1 is produced advanced purification process method and additive, it is characterized in that: No. 2 additives are the polyacrylamide of non-ionic type molecular weight about 8,000,000, be mixed with the 1g/L aqueous solution, by 2～2.5 liters of interpolations of every cubic metre of qualifying liquid, every cubic metre of qualifying liquid 1Kg(of ammonium sulphite addition contains SO
20.4～0.5g/L).
6. High pure no-Se electrolyzed metal Mn according to claim 1 is produced advanced purification process method and additive, it is characterized in that: when newly slotting, qualified additional liquid requirement is: Mn
2+34g/L, (NH
4)
2SO
4130g/L, SO
20.5g/L, No. 2 additive 2.0mg/L, PH6.6
The control parameter is in the electrolysis production process: tank liquor (negative electrode) Mn
2+12～14g/L, tank liquor pH value 7.5～8.0,34～37 ℃ of groove temperature.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436915A (en) * | 2013-09-23 | 2013-12-11 | 益阳金能新材料有限责任公司 | Electrolysis additive used for producing electrolytic manganese metal and mixed liquor thereof as well as preparation method of mixed liquor |
| CN105154917A (en) * | 2015-10-09 | 2015-12-16 | 靖西县大锰新材料有限公司 | Production method for 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 |
| CN108441888A (en) * | 2018-05-15 | 2018-08-24 | 江西理工大学 | A kind of tin electrorefining electrolyte compound additive |
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| US4149944A (en) * | 1977-04-04 | 1979-04-17 | Union Carbide Corporation | Method for electrolytic deposition of manganese |
| US4478697A (en) * | 1982-08-03 | 1984-10-23 | Kerr-Mcgee Chemical Corporation | Method for electrodepositing metallic manganese |
| CN102296323A (en) * | 2010-06-22 | 2011-12-28 | 陈榜龙 | Manufacturing system for producing electrolytic manganese metal by two-ore method |
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2013
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| US4149944A (en) * | 1977-04-04 | 1979-04-17 | Union Carbide Corporation | Method for electrolytic deposition of manganese |
| US4478697A (en) * | 1982-08-03 | 1984-10-23 | Kerr-Mcgee Chemical Corporation | Method for electrodepositing metallic manganese |
| CN102296323A (en) * | 2010-06-22 | 2011-12-28 | 陈榜龙 | Manufacturing system for producing electrolytic manganese metal by two-ore method |
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|---|
| 余逊贤等: "《锰》", 31 October 1980, 冶金工业部长沙黑色冶金矿山设计研究院 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436915A (en) * | 2013-09-23 | 2013-12-11 | 益阳金能新材料有限责任公司 | Electrolysis additive used for producing electrolytic manganese metal and mixed liquor thereof as well as preparation method of mixed liquor |
| CN103436915B (en) * | 2013-09-23 | 2016-03-23 | 益阳金能新材料有限责任公司 | For the preparation method of electrolysis additive, its mixed solution and mixed solution thereof that electrolytic metal Mn is produced |
| CN105154917A (en) * | 2015-10-09 | 2015-12-16 | 靖西县大锰新材料有限公司 | Production method for 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 |
| CN108441888A (en) * | 2018-05-15 | 2018-08-24 | 江西理工大学 | A kind of tin electrorefining electrolyte compound additive |
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Application publication date: 20130522 |