CN101538650A - Method for wet-separation of manganese from lead and silver in electrolytic-zinc anode slime - Google Patents
Method for wet-separation of manganese from lead and silver in electrolytic-zinc anode slime Download PDFInfo
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- CN101538650A CN101538650A CN200910043201A CN200910043201A CN101538650A CN 101538650 A CN101538650 A CN 101538650A CN 200910043201 A CN200910043201 A CN 200910043201A CN 200910043201 A CN200910043201 A CN 200910043201A CN 101538650 A CN101538650 A CN 101538650A
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- anode sludge
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Abstract
The invention relates to a method for the wet-separation of manganese from lead and silver in electrolytic-zinc anode slime. The method comprises the following concrete steps: firstly, pre-treating the electrolytic-zinc anode slime; secondly, carrying out the oxidation-reduction reaction by adding the electrolytic-zinc anode slime and reducing agent to a water solution containing sulfuric acid, wherein, manganese oxide in the anode slime is reduced and dissolved into manganese sulfate and the reducing agent is oxidized into sulfates, so that the solid manganese oxide in the anode slime is completely dissolved into the solution and the metal or the compounds of lead and silver in a solid form are retained in the residue; and thirdly, effectively separating manganese from lead and silver by solution/residue separation. By selecting sulfides as the reducing agent, the invention has the advantages of reliable material source, rapid reaction, no introduction of interference elements and the like; and then, the oxidation-reduction reaction has good chemical driving force and the reaction is rapid under the atmospheric pressure, so that lead and silver in the anode slime can be fully enriched, and the metal recovery rate reaching 95% to 99% is much higher than the lead and silver recovery rate of the conventional process for re-dissolving zinc in anode slime.
Description
Technical field
The present invention relates to a kind of anode sludge method for wet separation, particularly a kind of electrolytic zinc anode sludge wet separation manganese and plumbous silver-colored method.
Background technology
The main component of the electrolytic zinc anode sludge is a Manganse Dioxide; zinc hydrometallurgy factory generally all is that the zinc electrolysis anode sludge that will be main component turns back to zinc leaching operation with Manganse Dioxide; one of its purpose is to make wherein manganese oxide play the effect of oxygenant; help improving the difficult leaching yield of soaking zinc sulfide mineral of part in the calcining; two of purpose is to help removing iron too much in the leach liquor; improve electric zinc quality; three of purpose is after making solid-state manganese oxide be reduced to liquid manganous sulfate and entering into electrowinning process; the lead-silver anode plate is played a protective role; slow down the corrosion dissolution speed of positive plate, prolong the work-ing life of positive plate.The fluorine-containing chlorine of the raw material of some zinc smeltery is higher, and the electrolytic lead-silver anode plate of its zinc corrosion dissolution is very fast, contains higher lead and silver-colored in its anode sludge.Along with the value of non-ferrous metal and precious metal improves constantly, plumbous and silver-colored high efficiente callback problem should cause our great attention in plumbous and the electrolytic zinc anode sludge that silver content is higher.
Less to the manganese that the electrolytic zinc anode sludge is carried out with plumbous silver-colored isolating experimental study work, consult domestic literature, do not have to find that the manganese that the electrolytic zinc anode sludge is carried out separates the patent application of aspect with plumbous silver, only find 1 piece of pertinent literature report, Guangzhou Research Institute of Nonferrous Metals Wang Miao gives birth to and waits the people to adopt the art breading electrolytic zinc anode sludge of pyrogenic process+wet method, with brown coal as reductive agent, by high-temperature roasting 4 valency manganese are reduced to bivalent manganese, leach manganese with sulfuric acid again, plumbous silver is stayed in the leached mud, and realizes manganese and plumbous silver-colored separating.
Summary of the invention
The object of the present invention is to provide a kind of full wet processing electrolytic zinc anode sludge, realize manganese and the effective isolating method of plumbous silver.
Technical scheme of the present invention realizes by following approach, and the first step is carried out pre-treatment with the electrolytic zinc anode sludge; Second step, redox reaction leaches manganese, being about to the electrolytic zinc anode sludge and reductive agent adds and carries out redox reaction in the vitriolated aqueous solution, manganese oxide reduction of dissolved in the anode sludge is a manganous sulfate, reductive agent is oxidized to element and vitriol, thereby make the whole dissolvings of solid oxide manganese in the anode sludge enter solution, metal or compound plumbous and silver are stayed in the slag with solid-state form; In the 3rd step, manganese liquid separates with plumbous silver-colored slag, and the solution by adopting filter or pressure filter realization sulfur acid manganese separates with the slag of leaded silver.
Beneficial effect of the present invention, at first be that the present invention selects sulfide to make reductive agent, have from the horse's mouth, reaction is fast, cost is low, do not bring advantages such as interference element into, next is that redox reaction of the present invention has good chemical impellent, depress enough fast speed of response at natural atmosphere, do not need to take the measure of pressurizeing or reducing pressure, the 3rd is that the present invention passes through redox reaction, makes the plumbous silver in the anode sludge obtain abundant enrichment, and plumbous silver is common associated metal, later separation reclaims technical maturity, production cost is low, and metal recovery rate is up to 95-99%, and it is much higher to return the plumbous silver raising recovery rate of solving zinc operation than traditional anode sludge.
Embodiment
Describe the specific embodiment of the present invention below in detail.
The first step: the electrolytic zinc anode sludge is carried out pre-treatment;
Because the electrolytic zinc anode sludge will be carried the zinc sulfate of 1-4% inevitably secretly, so will carry out pre-treatment, the zinc sulfate water elution that is about to wherein removes.Can make by pre-treatment that zinc sulfate content is less than 0.5% in the anode sludge after the processing.This washing lotion can directly be returned the electrolytic zinc production system, also can do the raw material of other zinc product.The all or part of electrolytic zinc production system that directly is sent to of the manganese sulfate solution that redox reaction obtains is the minimum mode of processing cost, has both satisfied the needs of electrolytic zinc system increase mn ion, the following process expense of having removed manganese sulfate solution again from.
Second step: redox reaction leaches manganese
The main chemical reactions formula is as follows:
4MnO
2+MS+8H
+＝4Mn
2++MSO
4+4H
2O，
MnO
2+SO
2+＝Mn
2++SO
2- 4
The electrolytic zinc ANODE SLIME TREATMENT is made dissolve medium with sulfuric acid, and is identical with the medium of electrolytic zinc, do not bring new impurity element into, helps the further processing of subsequent products.Vitriolic beginning acid concentration can be selected in 5～30% scope.
The present invention selects sulfide to make reductive agent, and best reductive agent is a lead sulfide, and the reaction product lead sulfate exists with solid-state, can separate with liquid sulfuric acid manganese smoothly.And the lead sulfide that not exclusively stays of reaction is with solid-state form and lead sulfate coexistence, and next step does the plumbous processing of refining, do not have difficulties and bothers.The compound of argent in the anode sludge and silver is all stayed in the lead skim with solid-state, and high efficiency separation reclaims silver when helping the smelting of subsequent handling lead.The add-on of reductive agent is the 1.05-1.5% of theoretical amount.
If the reaction product manganese sulfate solution is directly to return the electrolytic zinc production system, is economically viable with zinc sulphide as reductive agent, become solution of zinc sulfate after the zinc sulphide reaction, enter the electrolytic zinc system with manganous sulfate, zinc sulfate is the main component of zinc electrolyte just.
The pulp density of redox reaction of the present invention is meant the solids content in the dilution heat of sulfuric acid.Concentration is too rare, and then reaction volume is huge, the production cost height; Concentration is too high, and then redox reaction is incomplete.So pulp density is more suitable in the scope of 10-35%.
Redox reaction service temperature of the present invention can be selected in 50～100 ℃ scope, and its speed of response is directly proportional with service temperature.In order to guarantee enough fast speed of response, service temperature is to be not less than 60 ℃ for well, and the time of reaction is 1～5 hour.
The 3rd step: manganese (liquid)/lead silver (slag) separates.
The solution of employing filter or pressure filter realization sulfur acid manganese separates with the slag of leaded silver.
The whereabouts of redox reaction product and subsequent treatment cost are that technology of the present invention needs the important step paid close attention in specific implementation process.Consider from the requirement of long-term scale operation, the liquid product manganous sulfate that obtains of reaction is with after the silver-colored slag of lead separates, reoxidizing and obtaining solid-state manganese dioxide product is the preferential processing mode of selecting, solid-state Manganse Dioxide both can have been made the leaching oxygenant that electrolytic zinc is produced, and also can directly sell as a kind of product.The all or part of electrolytic zinc production system that directly is sent to of the manganese sulfate solution that redox reaction obtains is the minimum mode of processing cost.The needs of electrolytic zinc system increase mn ion had both been satisfied, the following process expense of having removed manganese sulfate solution again from.The manganese sulfate solution that redox reaction obtains can pass through condensing crystal, the solid-state manganese sulfate product of output.
Several specific embodiments:
Example 1: certain factory's electrolytic zinc anode sludge contains Mn34.2%, Pb11.4%, Ag1250g/t, Zn2.3%.After three grades of washings of moisture, the anode sludge contains zinc and drops to 0.08%.With the dilution heat of sulfuric acid is medium, makees reductive agent, the anode sludge with lead sulfide breeze leaded 52.10%, silver-colored 234g/t: reductive agent=1: 2, and the slag rate that obtains is 70.3%, wherein contains Mn 0.1%, Pb 52.9%, Ag 774g/t; Obtain containing the solution of Mn 38.8g/l.
Example 2: certain factory's electrolytic zinc anode sludge contains Mn37.1%, Pb10.6%, Ag1107g/t, Zn3.06%.After three grades of washings of moisture, the anode sludge contains zinc and drops to 0.09%.With the dilution heat of sulfuric acid is medium, and with leaded 55.8%, the lead sulfide breeze of argentiferous 859g/t is made reductive agent, the anode sludge: reductive agent=1: 2, and the slag rate that obtains is 69.8%, wherein contains Mn 0.3%, Pb 55.9%, Ag1301.3g/t; Obtain containing Mn 43.6g/l solution.
Example 3: certain factory's electrolytic zinc anode sludge contains Mn34.2%, Pb11.4%, Ag1250g/t, Zn2.3%.With the dilution heat of sulfuric acid is medium, and leaded 8.9% with containing zinc 45.3%, the zinc sulphide breeze of argentiferous 85g/t is made reductive agent, the anode sludge: reductive agent=1.35: 1, the slag rate that obtains is 31.3%, wherein contains Mn 0.05%, Zn4.5%, Pb 32.9%, Ag 2341g/t; Obtain containing Mn 50.3g/l, the solution of Zn49.2g/l.
Example 4: certain factory's electrolytic zinc anode sludge contains Mn37.1%, Pb10.6%, Ag1107g/t, Zn3.06%.With the dilution heat of sulfuric acid is medium, with containing zinc 46.6%, and Pb3.78%, the zinc sulfide ore of Ag123.4g/t is made reductive agent, the anode sludge: reductive agent=1.35: 1, the slag rate that obtains is 29.5%, wherein contains Mn 0.23%, Pb 30.2%, Ag 2785g/t, and Zn 5.12%; Obtain containing Mn 57.6g/l, Zn 54.8g/l solution.
Claims (9)
1, a kind of electrolytic zinc anode sludge wet separation manganese and plumbous silver-colored method is characterized in that its concrete steps are:
The first step is carried out pre-treatment with the electrolytic zinc anode sludge;
Second step, redox reaction leaches manganese, being about to the electrolytic zinc anode sludge and reductive agent adds and carries out redox reaction in the vitriolated aqueous solution, manganese oxide reduction of dissolved in the anode sludge is a manganous sulfate, reductive agent is oxidized to element and vitriol, thereby make the whole dissolvings of solid oxide manganese in the anode sludge enter solution, metal or compound plumbous and silver are stayed in the slag with solid-state form;
In the 3rd step, manganese liquid separates with plumbous silver-colored slag, and the solution by adopting filter or pressure filter realization sulfur acid manganese separates with the slag of leaded silver.
2, the method for a kind of electrolytic zinc anode sludge wet separation manganese according to claim 1 and plumbous silver is characterized in that described pre-treatment is that the zinc sulfate that will carry secretly in the anode sludge washes with water and removes.
3, a kind of electrolytic zinc anode sludge wet separation manganese according to claim 1 and plumbous silver-colored method is characterized in that the described vitriolated aqueous solution, and its vitriolated beginning acid concentration is 5～30%.
4, a kind of electrolytic zinc anode sludge wet separation manganese according to claim 1 and plumbous silver-colored method is characterized in that described reductive agent is a sulfide.
5, a kind of electrolytic zinc anode sludge wet separation manganese according to claim 1 and plumbous silver-colored method is characterized in that described redox reaction is to depress at natural atmosphere to carry out, and do not need pressurization or decompression.
6, a kind of electrolytic zinc anode sludge wet separation manganese according to claim 1 and plumbous silver-colored method, the pulp density that it is characterized in that described redox reaction is 10-35%.
7, a kind of electrolytic zinc anode sludge wet separation manganese according to claim 1 and plumbous silver-colored method is characterized in that the service temperature of described redox reaction is controlled in 50～100 ℃ of scopes, and the time of reaction is 1～5 hour.
8, according to claim 1,4 described a kind of electrolytic zinc anode sludge wet separation manganese and plumbous silver-colored method, it is characterized in that described reductive agent adopts lead sulfide or zinc sulphide.
9, according to claim 1,4 described a kind of electrolytic zinc anode sludge wet separation manganese and plumbous silver-colored method, the add-on that it is characterized in that described reductive agent is the 1.05-1.5% of theoretical amount.
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|---|---|---|---|
| CN200910043201A CN101538650A (en) | 2009-04-24 | 2009-04-24 | Method for wet-separation of manganese from lead and silver in electrolytic-zinc anode slime |
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| CN200910043201A CN101538650A (en) | 2009-04-24 | 2009-04-24 | Method for wet-separation of manganese from lead and silver in electrolytic-zinc anode slime |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002584A (en) * | 2010-11-04 | 2011-04-06 | 株洲冶炼集团股份有限公司 | Method of recovering manganese, lead and silver from zinc electrolyzed anode mud by utilizing acid-making tail gas |
| CN102168177A (en) * | 2011-04-13 | 2011-08-31 | 济源市东方化工有限责任公司 | Method for directly leaching electrolytic zinc anode mud manganese dioxide |
| CN102586599A (en) * | 2012-03-07 | 2012-07-18 | 株洲冶炼集团股份有限公司 | Method for recovering valued metals from zinc anode sludge |
| CN102912138A (en) * | 2012-10-19 | 2013-02-06 | 湖南有色金属研究院 | Method of recycling zinc, manganese, lead and silver from zinc electrowinning anode mud |
| CN104591291A (en) * | 2015-01-08 | 2015-05-06 | 杜新玲 | Method for producing manganese sulfate by performing zinc electrodeposit anode slime treatment on sulfur dioxide flue gas |
| CN105907960A (en) * | 2016-04-22 | 2016-08-31 | 王树立 | Method for combined resourceful treatment of lead concentrate and zinc anode mud |
| CN106544511A (en) * | 2016-12-12 | 2017-03-29 | 株洲冶炼集团股份有限公司 | A kind of method of synthetical recovery manganese, lead, silver and selenium from Manganese anode slime |
| CN107245579A (en) * | 2017-04-28 | 2017-10-13 | 贵州宏达环保科技有限公司 | A kind of method that Zn, Mn, Pb, Ag are extracted in the earth of positive pole from zinc electrolysis |
| CN108277353A (en) * | 2018-03-19 | 2018-07-13 | 六盘水中联工贸实业有限公司 | A method of recycling manganese from the zinc electrolysis earth of positive pole |
| CN108754145A (en) * | 2018-05-30 | 2018-11-06 | 宁夏天元锰业有限公司 | The technique of valuable metal in a kind of recycling electrolytic manganese anode mud |
| CN108823410A (en) * | 2018-06-01 | 2018-11-16 | 青海华信环保科技有限公司 | A method of feed grade manganese sulfate and recycling lead are prepared with electrolytic zinc anode mud |
| CN109402406A (en) * | 2018-12-26 | 2019-03-01 | 湖南稀土金属材料研究院 | The method of valuable metal is recycled from zinc anode sludge |
| CN111850305A (en) * | 2020-07-28 | 2020-10-30 | 昆明理工大学 | Method for leaching cobalt and manganese from manganese-rich cobalt slag |
| CN113355522A (en) * | 2021-06-11 | 2021-09-07 | 邵阳学院 | Comprehensive recovery processing method for zinc anode mud |
| CN115011799A (en) * | 2022-07-13 | 2022-09-06 | 重庆上甲电子股份有限公司 | Method for producing soft magnetic trimanganese tetroxide by using electrolytic manganese anode slime |
| EP4146411A4 (en) * | 2020-05-07 | 2024-06-05 | Befesa Zinc Metal LLC | A method, a system, and an apparatus for preparing manganese sulfate |
-
2009
- 2009-04-24 CN CN200910043201A patent/CN101538650A/en active Pending
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002584A (en) * | 2010-11-04 | 2011-04-06 | 株洲冶炼集团股份有限公司 | Method of recovering manganese, lead and silver from zinc electrolyzed anode mud by utilizing acid-making tail gas |
| CN102168177A (en) * | 2011-04-13 | 2011-08-31 | 济源市东方化工有限责任公司 | Method for directly leaching electrolytic zinc anode mud manganese dioxide |
| CN102586599A (en) * | 2012-03-07 | 2012-07-18 | 株洲冶炼集团股份有限公司 | Method for recovering valued metals from zinc anode sludge |
| CN102586599B (en) * | 2012-03-07 | 2013-07-31 | 株洲冶炼集团股份有限公司 | Method for recovering valued metals from zinc anode sludge |
| CN102912138A (en) * | 2012-10-19 | 2013-02-06 | 湖南有色金属研究院 | Method of recycling zinc, manganese, lead and silver from zinc electrowinning anode mud |
| CN104591291A (en) * | 2015-01-08 | 2015-05-06 | 杜新玲 | Method for producing manganese sulfate by performing zinc electrodeposit anode slime treatment on sulfur dioxide flue gas |
| CN104591291B (en) * | 2015-01-08 | 2016-06-15 | 杜新玲 | One utilizes Zinc electrolysis ANODE SLIME TREATMENT sulfur dioxide flue gas to produce manganese sulfate method |
| CN105907960A (en) * | 2016-04-22 | 2016-08-31 | 王树立 | Method for combined resourceful treatment of lead concentrate and zinc anode mud |
| CN106544511B (en) * | 2016-12-12 | 2018-05-04 | 株洲冶炼集团股份有限公司 | A kind of synthetical recovery manganese from Manganese anode slime, lead, the method for silver and selenium |
| CN106544511A (en) * | 2016-12-12 | 2017-03-29 | 株洲冶炼集团股份有限公司 | A kind of method of synthetical recovery manganese, lead, silver and selenium from Manganese anode slime |
| CN107245579B (en) * | 2017-04-28 | 2019-03-05 | 贵州宏达环保科技有限公司 | A method of extracting Zn, Mn, Pb, Ag from the zinc electrolysis earth of positive pole |
| CN107245579A (en) * | 2017-04-28 | 2017-10-13 | 贵州宏达环保科技有限公司 | A kind of method that Zn, Mn, Pb, Ag are extracted in the earth of positive pole from zinc electrolysis |
| CN108277353A (en) * | 2018-03-19 | 2018-07-13 | 六盘水中联工贸实业有限公司 | A method of recycling manganese from the zinc electrolysis earth of positive pole |
| CN108277353B (en) * | 2018-03-19 | 2019-08-13 | 六盘水中联工贸实业有限公司 | A method of recycling manganese from the zinc electrolysis earth of positive pole |
| CN108754145A (en) * | 2018-05-30 | 2018-11-06 | 宁夏天元锰业有限公司 | The technique of valuable metal in a kind of recycling electrolytic manganese anode mud |
| CN108754145B (en) * | 2018-05-30 | 2019-09-17 | 宁夏天元锰业有限公司 | The technique of valuable metal in a kind of recycling electrolytic manganese anode mud |
| CN108823410A (en) * | 2018-06-01 | 2018-11-16 | 青海华信环保科技有限公司 | A method of feed grade manganese sulfate and recycling lead are prepared with electrolytic zinc anode mud |
| CN109402406A (en) * | 2018-12-26 | 2019-03-01 | 湖南稀土金属材料研究院 | The method of valuable metal is recycled from zinc anode sludge |
| CN109402406B (en) * | 2018-12-26 | 2020-11-03 | 湖南稀土金属材料研究院 | Method for recovering valuable metal from zinc anode mud |
| EP4146411A4 (en) * | 2020-05-07 | 2024-06-05 | Befesa Zinc Metal LLC | A method, a system, and an apparatus for preparing manganese sulfate |
| CN111850305A (en) * | 2020-07-28 | 2020-10-30 | 昆明理工大学 | Method for leaching cobalt and manganese from manganese-rich cobalt slag |
| CN113355522A (en) * | 2021-06-11 | 2021-09-07 | 邵阳学院 | Comprehensive recovery processing method for zinc anode mud |
| CN115011799A (en) * | 2022-07-13 | 2022-09-06 | 重庆上甲电子股份有限公司 | Method for producing soft magnetic trimanganese tetroxide by using electrolytic manganese anode slime |
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