CN102094119A - Method for preparing electrolytic manganese metal with low-grade pyrolusite wet leaching - Google Patents
Method for preparing electrolytic manganese metal with low-grade pyrolusite wet leaching Download PDFInfo
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- CN102094119A CN102094119A CN2011100305612A CN201110030561A CN102094119A CN 102094119 A CN102094119 A CN 102094119A CN 2011100305612 A CN2011100305612 A CN 2011100305612A CN 201110030561 A CN201110030561 A CN 201110030561A CN 102094119 A CN102094119 A CN 102094119A
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Abstract
The invention discloses a method for preparing electrolytic manganese metal with low-grade pyrolusite wet leaching, which comprises the following steps of: after low-grade pyrolusite is crushed and screened, mixing slurry with electrolytic manganese anolyte, adding sulfuric acid to control acidity, and reducing high-valent manganese insoluble in water into low-valent manganese readily soluble in water through a redox reaction by using reduced iron powder or waste iron scraps as a reducing agent; controlling certain acidity, reaction temperature and time, stirring and leaching, and then precipitating and filtering; purifying, decontaminating and separating a filter liquor to obtain a pure manganese sulfate solution; and electrolyzing the manganese sulfate solution to obtain an electrolytic manganese product, wherein the leaching rate of manganese is higher than 98%, the recovery rate of manganese is higher than 90%, and the purity of electrolytic manganese metal is higher than 99.8%. The method has the advantages that the raw materials of the reducing agent have wide sources and low price, the reaction time is short, the conditions of the leaching process are mild, the leaching rate of manganese is high, the purification process is simple, and the process route of the present carbonic acid manganese ore for preparing electrolytic manganese metal is not changed.
Description
Technical field
The present invention relates to a kind of is that the raw material wet method leaches the method for preparing electrolytic metal Mn with low-grade pyrolusite.
Background technology
China's manganese resource is many and not rich, finds out 6.4 hundred million tons of resource reserves, and secondly ore type is manganese oxide ore and ferrimanganic ore deposit based on manganese carbonate ore, and the overwhelming majority is a poor manganese ore, and rich manganese ore only accounts for the 6-8% of whole resource reserves.With the carbonic acid ore deposit is raw material production electrolytic manganese technology maturation, occupies the leading level in the world, is extensively adopted by domestic enterprise.Along with exploitation for many years, China's manganese ore abundant ore source falls sharply.Current, the poorness of manganese resource is just restricting production and the Sustainable development that China's manganese is product.In the area that some electrolytic metal Mn products productions of China are concentrated, the grade of the manganese carbonate ore that uses is reduced to and has only 10-15% by containing manganese 18-20%.And on the other hand, because the smelting difficulty of low-grade pyrolusite is big, the rate of recovery is low, the reduction process cost is too high, no matter what adopt is existing thermal process or wet processing, all be difficult to the valuable metal in the economic recovery ore, economic benefit all is subjected to ore to contain the manganese grade to restrict, thereby causes the pyrolusite that contains manganese 20-25% in a large number to be not used.Thereby in the electrolytic manganese production field, the utilization of low-grade pyrolusite is still a blank, how to utilize low-grade pyrolusite to produce electrolytic metal Mn, particularly solve the technical problem of its this bottleneck of reducing process, the comprehensive utilization ratio that improves resource is a problem that needs to be resolved hurrily, and also is the target that electrolytic metal Mn enterprise is pursued.This is to alleviating the current manganese resource of China contradiction in short supply, guaranteeing that the Sustainable development of electrolytic manganese industry has crucial strategic importance.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with low-grade pyrolusite, adopts the wet reducing extract technology to prepare the method for electrolytic metal Mn.
The present invention be with low-grade pyrolusite behind crushing and screening, size mixing with the electrolytic manganese anolyte, add the sulfuric acid controlling acidity, as reductive agent, make the high oxidation state manganese that is insoluble in water be reduced to low-oxidation-state manganese soluble in water through redox reaction with reduced iron powder or waste iron filing.Control certain acidity, temperature of reaction and the time, agitation leach is carried out sedimentation then and is filtered.Filtrate obtains pure manganese sulfate solution after purification and impurity removal separates, manganese sulfate solution is carried out electrolytic preparation obtain the electrolytic manganese product.
Implementation step of the present invention is as follows:
Low-grade pyrolusite is pulverized the 50-300 order, with the 2-10 of pyrolusite quality 10% sulfuric acid or electrolytic manganese anolyte modulation ore pulp doubly, the 0.1-0.5 that adds the pyrolusite quality in the ore pulp doubly reduced iron powder or waste iron filing as reductive agent, under 50-95 ℃ of temperature, constantly obtained reacting leach liquor in stirring reaction 0.5-4 hour, it is 2.0-3.0 that the reaction leach liquor is adjusted agent adjusting pH with acidity, it is ammoniacal liquor that acidity is adjusted agent, when regulating the pH value with ammoniacal liquor, as the ammonium sulfate concentrations of the generation that neutralizes then replaces ammoniacal liquor to regulate the pH value with manganese carbonate ore or manganous carbonate above the concentration 120-140g/L that electrolytic manganese process allowed; Add H then
2O
2With Fe
2+Be oxidized to Fe
3+, stir and purify 1-2 hour, remove heavy metal ion such as de-iron, to filter and obtain leach liquor, filtrate is used the SDD deep impurity-removing, transfers pH to 5.0-6.7 with ammoniacal liquor, carries out the electrolysis production electrolytic metal Mn more according to a conventional method.The leaching yield of manganese is greater than 98%, and the purity of electrolytic metal Mn is greater than 99.8%, and the rate of recovery of manganese is greater than 90%.
The present invention adopts full wet processing, reduces energy consumption, reduces environmental pollution, improves resource utilization, realizes cleaner production.The reductive agent raw material sources are extensive, cheap, reaction times is short, the extract technology mild condition, the leaching yield height of manganese, scavenging process is simple, and does not change existing manganese carbonate ore and prepare the electrolytic metal Mn operational path, has opened up the raw material sources of manganese oxide ore class for the production of electrolytic manganese, thereby alleviate manganese carbonate ore situation in short supply, have environmental protection and economic double benefit.
Embodiment:
Embodiment one:
With manganese content is that 28.86% pyrolusite is pulverized 100 orders (forming as shown in table 1), dilution heat of sulfuric acid modulation ore pulp with 4 times 10% of pyrolusite, add the waste iron filing (iron level 90%) of 0.20 times of pyrolusite quality in the ore pulp, obtained reacting leach liquor in 2 hours at 90 ℃ of following stirring reactions; It is 2.0-3.0 that leach liquor is neutralized to pH with manganous carbonate or ammoniacal liquor as acidity regulator, adds an amount of H
2O
2With Fe
2+Be oxidized to Fe
3+, stir and purify 1 hour, filter and obtain leach liquor.Leach liquor after deironing is qualified is further removed heavy metal ion impurities in the solution with SDD, transfers pH to 6.7 with ammoniacal liquor, regulates ammonium sulfate concentrations, and electrolytic manganese process carries out electrolysis routinely.The leaching yield of manganese is 98.5%, and the purity of electrolytic metal Mn is 99.85%, the rate of recovery 95% of manganese.
Table 1 pyrolusite component list
Embodiment two:
With manganese content is that 28.86% pyrolusite is pulverized 120 orders (forming as shown in table 1), with the electrolytic manganese anolyte modulation ore pulp of 5 times of pyrolusites.Add the reduced iron powder (iron content 85%) of 0.3 times of pyrolusite quality in the ore pulp, obtained reacting leach liquor in 2 hours at 95 ℃ of following stirring reactions.It is 2.0-3.0 that leach liquor is neutralized to pH with manganous carbonate as acidity regulator, adds an amount of H
2O
2With Fe
2+Be oxidized to Fe
3+, stir and purify 1 hour, filter and obtain leach liquor.Leach liquor after deironing is qualified is further removed heavy metal ion impurities in the solution with SDD, transfers pH to 6.5 with ammoniacal liquor, regulates ammonium sulfate concentrations, and electrolytic manganese process carries out electrolysis routinely.The leaching yield of manganese is 98.8%, and the purity of electrolytic metal Mn is 99.86%, the rate of recovery 95.3% of manganese.
Embodiment three:
With manganese content is that 28.86% pyrolusite is pulverized 80 orders (forming as shown in table 1), with the electrolytic manganese anolyte modulation ore pulp of 4.5 times of pyrolusites.Add the waste iron filing (iron content 90%) of 0.25 times of pyrolusite quality in the ore pulp, obtained reacting leach liquor in 2 hours at 90 ℃ of following stirring reactions.It is 2.0-3.0 that leach liquor is neutralized to pH with ammoniacal liquor as acidity regulator, adds an amount of H
2O
2With Fe
2+Be oxidized to Fe
3+, stir and purify 1 hour, filter and obtain leach liquor.Leach liquor after deironing is qualified is further removed heavy metal ion impurities in the solution with SDD, transfers pH to 6.6 with ammoniacal liquor, carries out electrolysis according to a conventional method.The leaching yield of manganese is 98.8%, and the purity of electrolytic metal Mn is 99.88%, the rate of recovery 95.5% of manganese.
Claims (3)
1. a low-grade pyrolusite wet method leaches the method for preparing electrolytic metal Mn, it is characterized in that low-grade pyrolusite is pulverized the 50-300 order, with the 2-10 of pyrolusite quality 10% sulfuric acid or electrolytic manganese anolyte modulation ore pulp doubly, the 0.1-0.5 that adds the pyrolusite quality in the ore pulp doubly reduced iron powder or waste iron filing as reductive agent, under 50-95 ℃ of temperature, constantly obtained reacting leach liquor in stirring reaction 0.5-4 hour, it is 2.0-3.0 that the reaction leach liquor is adjusted agent adjusting pH with acidity, adds H
2O
2With Fe
2+Be oxidized to Fe
3+, stir and purify 1-2 hour, remove heavy metal ion such as de-iron, to filter and obtain leach liquor, filtrate is used the SDD deep impurity-removing, transfers pH to 5.0-6.7 with ammoniacal liquor, carries out the electrolysis production electrolytic metal Mn more according to a conventional method.
2. a kind of low-grade pyrolusite wet method according to claim 1 leaches the method for preparing electrolytic metal Mn, it is characterized in that described low-grade pyrolusite is a manganese content greater than 15% pyrolusite.
3. a kind of low-grade pyrolusite wet method according to claim 1 leaches the method for preparing electrolytic metal Mn, it is characterized in that it is ammoniacal liquor or manganese carbonate ore or manganous carbonate that described acidity is adjusted agent.
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Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102605187A (en) * | 2011-10-10 | 2012-07-25 | 云南建水锰矿有限责任公司 | Method for producing manganese sulfate by manganese-rich slag through pressure leaching |
| CN102888510A (en) * | 2012-10-24 | 2013-01-23 | 广西天鸿鑫锰业科技有限公司 | Method for preparing manganese sulfate solution from low-grade manganese oxide by reducing leaching at normal temperature and pressure |
| CN103205570A (en) * | 2013-04-26 | 2013-07-17 | 吉首大学 | Method for producing vanadium pentoxide and by-product manganese sulfate from by using coal vanadium ore and pyrolusite together |
| CN103526018A (en) * | 2013-10-17 | 2014-01-22 | 桂林翔云锰业有限责任公司 | Method for producing electrolytic manganese from manganese carbonate ore with low manganese content and high iron content |
| CN103627900A (en) * | 2013-10-31 | 2014-03-12 | 中信大锰矿业有限责任公司大新锰矿分公司 | Method for removing impurities from manganese sulfate through total carbonic acid leaching |
| CN103757253A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching pyrolusite |
| CN103757429A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for re-leaching waste residue generated through leaching manganese carbonate ore with sulfuric acid |
| CN103757223A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching pyrolusite |
| CN103757208A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching manganese carbonate ore |
| CN103757269A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for re-leaching waste residue generated through leaching manganese carbonate ore with sulfuric acid |
| CN103757232A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching pyrolusite |
| CN103937973A (en) * | 2014-04-16 | 2014-07-23 | 广西民族大学 | Organic-inorganic combined pyrolusite reduction method |
| CN104016417A (en) * | 2014-06-10 | 2014-09-03 | 吉首大学 | Process for preparing electronic grade manganous-manganic oxide and byproduct nano-iron oxide red from pyrolusite |
| CN105779784A (en) * | 2016-03-18 | 2016-07-20 | 广州有色金属研究院 | Method for leaching gold and silver out of kustelite wrapped by manganese under normal pressure and temperature |
| CN106148734A (en) * | 2015-03-27 | 2016-11-23 | 汪云华 | A kind of ferrous sulfate that comprehensively utilizes produces the technology of electrolytic manganese |
| CN106756001A (en) * | 2016-12-29 | 2017-05-31 | 宁夏天元锰业有限公司 | A kind of method of the production electrolytic manganese metal for comprehensively utilizing electrolytic manganese residues |
| CN107699714A (en) * | 2017-09-19 | 2018-02-16 | 四川大学 | A kind of method that manganese sulfate electrolyte is prepared suitable for leaching pyrolusite by sulfur dioxide |
| CN110331284A (en) * | 2019-08-23 | 2019-10-15 | 贵州合众锰业科技有限公司 | A method of electrolytic manganese is prepared using pyrolusite |
| CN110396612A (en) * | 2019-08-29 | 2019-11-01 | 贵州大学 | A kind of method that pyrolusite reduction prepares manganese sulfate solution |
| CN110735155A (en) * | 2018-09-27 | 2020-01-31 | 庞炼红 | Method for producing electrolytic manganese metal and co-producing manganese dioxide |
| CN111111854A (en) * | 2019-12-30 | 2020-05-08 | 铜仁学院 | Manganese ore industrialization wet ball milling method based on electrolytic manganese metal system backwater |
| CN111304439A (en) * | 2020-03-31 | 2020-06-19 | 北京矿冶科技集团有限公司 | Method for recovering valuable metals from submarine manganese ore resources |
| CN113247877A (en) * | 2021-05-27 | 2021-08-13 | 广西锰华新能源科技发展有限公司 | Method for preparing battery-grade iron phosphate and manganese phosphate from manganese ore leaching residues |
| CN113684381A (en) * | 2021-08-27 | 2021-11-23 | 昆明理工大学 | Method for preparing high-purity manganese sulfate by microwave-flow field coupling strengthening treatment of pyrolusite |
| CN114262793A (en) * | 2020-09-16 | 2022-04-01 | 四川省平武锰业(集团)有限公司 | Method for preparing manganese by mixing sulfur-containing manganese carbonate ore and pyrolusite and leaching with acid |
| CN114457235A (en) * | 2022-01-26 | 2022-05-10 | 贵州金瑞新材料有限责任公司 | Application method of high-iron reduced ore in electrolytic manganese production process |
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| CN102605186A (en) * | 2011-10-10 | 2012-07-25 | 云南建水锰矿有限责任公司 | Method for producing manganese sulfate from manganese-rich slag through atmospheric pressure leaching |
| CN102605187A (en) * | 2011-10-10 | 2012-07-25 | 云南建水锰矿有限责任公司 | Method for producing manganese sulfate by manganese-rich slag through pressure leaching |
| CN102888510A (en) * | 2012-10-24 | 2013-01-23 | 广西天鸿鑫锰业科技有限公司 | Method for preparing manganese sulfate solution from low-grade manganese oxide by reducing leaching at normal temperature and pressure |
| CN103205570B (en) * | 2013-04-26 | 2015-07-29 | 吉首大学 | Bone coal navajoite and pyrolusite together produce the method for Vanadium Pentoxide in FLAKES by-product manganese sulfate |
| CN103205570A (en) * | 2013-04-26 | 2013-07-17 | 吉首大学 | Method for producing vanadium pentoxide and by-product manganese sulfate from by using coal vanadium ore and pyrolusite together |
| CN103526018A (en) * | 2013-10-17 | 2014-01-22 | 桂林翔云锰业有限责任公司 | Method for producing electrolytic manganese from manganese carbonate ore with low manganese content and high iron content |
| CN103627900A (en) * | 2013-10-31 | 2014-03-12 | 中信大锰矿业有限责任公司大新锰矿分公司 | Method for removing impurities from manganese sulfate through total carbonic acid leaching |
| CN103627900B (en) * | 2013-10-31 | 2015-08-19 | 中信大锰矿业有限责任公司大新锰矿分公司 | A kind of full carbonic acid leaching manganese sulfate impurity-removing method |
| CN103757208B (en) * | 2013-12-29 | 2015-11-25 | 四川师范大学 | The leaching method of manganese carbonate ore |
| CN103757208A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching manganese carbonate ore |
| CN103757269A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for re-leaching waste residue generated through leaching manganese carbonate ore with sulfuric acid |
| CN103757232A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching pyrolusite |
| CN103757223A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching pyrolusite |
| CN103757429A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for re-leaching waste residue generated through leaching manganese carbonate ore with sulfuric acid |
| CN103757253A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching pyrolusite |
| CN103757223B (en) * | 2013-12-29 | 2016-01-20 | 四川师范大学 | The leaching method of pyrolusite |
| CN103757232B (en) * | 2013-12-29 | 2016-02-24 | 四川师范大学 | The leaching method of pyrolusite |
| CN103937973A (en) * | 2014-04-16 | 2014-07-23 | 广西民族大学 | Organic-inorganic combined pyrolusite reduction method |
| CN104016417A (en) * | 2014-06-10 | 2014-09-03 | 吉首大学 | Process for preparing electronic grade manganous-manganic oxide and byproduct nano-iron oxide red from pyrolusite |
| CN104016417B (en) * | 2014-06-10 | 2016-02-03 | 吉首大学 | The nanometer iron oxide red technique of electronic-grade trimanganese tetroxide by-product prepared by pyrolusite |
| CN106148734A (en) * | 2015-03-27 | 2016-11-23 | 汪云华 | A kind of ferrous sulfate that comprehensively utilizes produces the technology of electrolytic manganese |
| CN105779784A (en) * | 2016-03-18 | 2016-07-20 | 广州有色金属研究院 | Method for leaching gold and silver out of kustelite wrapped by manganese under normal pressure and temperature |
| CN106756001A (en) * | 2016-12-29 | 2017-05-31 | 宁夏天元锰业有限公司 | A kind of method of the production electrolytic manganese metal for comprehensively utilizing electrolytic manganese residues |
| CN107699714A (en) * | 2017-09-19 | 2018-02-16 | 四川大学 | A kind of method that manganese sulfate electrolyte is prepared suitable for leaching pyrolusite by sulfur dioxide |
| CN110735155B (en) * | 2018-09-27 | 2021-06-22 | 庞炼红 | Method for producing electrolytic manganese metal and co-producing manganese dioxide |
| CN110735155A (en) * | 2018-09-27 | 2020-01-31 | 庞炼红 | Method for producing electrolytic manganese metal and co-producing manganese dioxide |
| CN110331284A (en) * | 2019-08-23 | 2019-10-15 | 贵州合众锰业科技有限公司 | A method of electrolytic manganese is prepared using pyrolusite |
| CN110396612A (en) * | 2019-08-29 | 2019-11-01 | 贵州大学 | A kind of method that pyrolusite reduction prepares manganese sulfate solution |
| CN111111854A (en) * | 2019-12-30 | 2020-05-08 | 铜仁学院 | Manganese ore industrialization wet ball milling method based on electrolytic manganese metal system backwater |
| CN111304439A (en) * | 2020-03-31 | 2020-06-19 | 北京矿冶科技集团有限公司 | Method for recovering valuable metals from submarine manganese ore resources |
| CN114262793A (en) * | 2020-09-16 | 2022-04-01 | 四川省平武锰业(集团)有限公司 | Method for preparing manganese by mixing sulfur-containing manganese carbonate ore and pyrolusite and leaching with acid |
| CN113247877A (en) * | 2021-05-27 | 2021-08-13 | 广西锰华新能源科技发展有限公司 | Method for preparing battery-grade iron phosphate and manganese phosphate from manganese ore leaching residues |
| CN113684381A (en) * | 2021-08-27 | 2021-11-23 | 昆明理工大学 | Method for preparing high-purity manganese sulfate by microwave-flow field coupling strengthening treatment of pyrolusite |
| CN114457235A (en) * | 2022-01-26 | 2022-05-10 | 贵州金瑞新材料有限责任公司 | Application method of high-iron reduced ore in electrolytic manganese production process |
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Application publication date: 20110615 |