CN101684562A - Liquid making technique for manganese oxide ore - Google Patents
Liquid making technique for manganese oxide ore Download PDFInfo
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- CN101684562A CN101684562A CN200810073819A CN200810073819A CN101684562A CN 101684562 A CN101684562 A CN 101684562A CN 200810073819 A CN200810073819 A CN 200810073819A CN 200810073819 A CN200810073819 A CN 200810073819A CN 101684562 A CN101684562 A CN 101684562A
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Abstract
The invention discloses a liquid making technique for manganese oxide ore, comprising the steps of: adding the manganese oxide ore powder, pyrite powder, sulfuric acid solution into a leaching vat forleaching; adding a neutralizing agent for neutralizing after reaching leaching termination; adding ammonia sulfate, potassium permanganate and sodium dimethyldithiocarbamate into the neutralization liquid after filtration until the nickel is qualitatively removed; then, adding barium sulfide or adding barium sulfide into the filtrate after filtration, wherein the dosage of barium sulfide is 100-2000g/m<3> manganese sulfate solution; adding XY-3 impurity removal agent after filtration, wherein the dosage of XY-3 impurity removal agent is 50-400g/m<3> manganese sulfate solution, the temperatureis controlled at 30-80 DEG C, the reaction time is 0.5-3h, and the pH is 4.5-6.9; and filtrating to obtained purified manganese sulfate solution. The recovery rate of the qualified, refined and purified manganese sulfate solution is more than 90%, based on common electrolytic technique, the quality of products achieves national standard, the electrolytic yield is larger than 3kg/veneer, the powerconsumption is not more than 7500kwh/t, and the yield, cost and efficiency are all better than the traditional level of manganous carbonate production.
Description
Technical field:
The present invention relates to a kind of liquid making technique of method, particularly a kind of manganese oxide ore of manganese smelting.
Background technology:
Electrolytic manganese is smelted and is developed into now, and China's electrolytic manganese production nearly all is to adopt manganese carbonate ore, because manganese carbonate ore dilution price is day by day progressively raised and caused the electrolytic manganese production cost progressively to strengthen, brings tremendous economic pressure for many enterprises.The low-grade manganese oxide ore of China is very abundant, and price is relatively low, is the preferred raw materials that substitutes low-grade manganese carbonate ore.The beginning of the nineties in last century, some manganese smelting enterprises began to adopt manganese oxide ore not have the baked for producing electrolytic manganese dioxide to achieve success.Afterwards, many enterprises attempt adopting manganese oxide ore not have the baked for producing electrolytic metal Mn in succession, at present the liquid making technique of manganese smelting industry manganese oxide ore is that reductive agents such as sulfuric acid or anolyte, manganese oxide ore, sulfurous iron ore are added in the leaching vat, after leaching the chemical combination end, neutralize again, again neutralizer is purified and be sent to electrowinning process after qualified, do not reach the state of the art that adopts manganous carbonate to produce electrolytic metal Mn in other words but all fail, its key issue is the system liquid quality of manganese oxide ore.
Summary of the invention:
The object of the present invention is to provide a kind of liquid making technique of manganese oxide ore, by the manganese sulfate solution that this technology makes, need only by existing electrolysis tech and just can realize that output, cost, the efficient of electrolytic manganese can reach the level that traditional employing manganous carbonate is produced electrolytic metal Mn at least.
Processing step of the present invention is:
1), manganese oxide powder, troilite powder, sulphuric acid soln or anolyte are put in the leaching vat, the process reaction temperature is controlled at 50～100 ℃, 1.5～6 hours time, manganese oxide powder, troilite powder, vitriolic weight ratio are 1: 0.09～0.40: 0.1～0.4, the reaction end sulfuric acid content is＜15g/l to obtain containing the leaching liquid of manganese 25～45g/l;
2), add neutralizing agent in the leaching liquid that obtains toward step 1) and neutralize, process temperature is controlled at 50～90 ℃, reaction is abandoned filter residue until pH value at 4.5～6.9 after-filtration, rough manganese sulfate solution;
3), get step 2) the rough manganese sulfate solution of gained, control its ammonium sulfate concentrations at 70～140g/l, add potassium permanganate, consumption is 10～100g/m
3Manganese sulfate solution after reacting completely, adds Sodium Dimethyldithiocarbamate, until remove nickel qualified till, add barium sulphide then or filter after in filtrate, add barium sulphide again, the barium sulphide consumption is 100g～2000g/m
3Manganese sulfate solution, process temperature is controlled at 30～80 ℃, reaction times is 0.5～3 hour, pH value is 4.5～6.9, filter to such an extent that slightly go on foot the purification manganese sulfate solution then, or get step 2) the rough manganese sulfate solution of gained, control its ammonium sulfate concentrations at 70～140g/l, add barium sulphide, the barium sulphide consumption is 100g～2000g/m
3Manganese sulfate solution, process temperature are controlled at 30～80 ℃, and the reaction times is 0.5～3 hour, and pH value filters the back and adds potassium permanganate 4.5～6.9, and consumption is 10～100g/m
3Manganese sulfate solution after reacting completely, adds Sodium Dimethyldithiocarbamate, till qualified except that nickel, filters to such an extent that slightly the step purifies manganese sulfate solution then;
4), get the step 3) gained and slightly go on foot the purification manganese sulfate solution, add the XY-3 cleaner, XY-3 cleaner consumption is 50g～400g/m
3The thick step purifies manganese sulfate solution, and process temperature is controlled at 30～80 ℃, and the reaction times is 0.5～3 hour, and pH value filters to such an extent that refining purification manganese sulfate solution uses for electrowinning process 4.5～6.9 then.
Above-mentioned four processes can independently be carried out successively;
Above-mentioned four processes also can be carried out successively continuously.
The qualified refining purification manganese sulfate solution that makes by technology of the present invention, the rate of recovery reaches＞and 90.%, electrolysis tech carries out electrolysis routinely, quality product is up to state standards, electrolysis output＞3kg/ veneer, power consumption≤7500kwh/ ton has realized that output, cost, the efficient of electrolytic manganese has surmounted the level that traditional employing manganous carbonate is produced electrolytic metal Mn.
If the system liquid operation that adopt leaching continuously, purifies, i.e. continuous dosing, output continuously, compare with traditional interruption leaching, purification process, the quantity of leaching vat and purification tank reduces about 50%, and operator's quantity and working strength of workers can be and significantly reduce, and output is multiplied.
Description of drawings:
Fig. 1 is a process flow diagram of the present invention.
Specific embodiment:
Embodiment 1:
Manganese oxide powder, troilite powder, vitriolic weight ratio are 1: 0.213: 0.36
1) squeeze into the anolyte of about 1/3rd volumes, earlier in the leaching vat, stirring simultaneously, the leaching vat effective volume is 180m
3, anolyte contains manganese 12.6g/l, sulfur acid 32.68g/l, has been preheated to about 80 ℃, squeeze into 6.072 tons in sulfuric acid then, drop into grade again and be 31 tons of 17% manganese oxide powders, squeeze into segment anode liquid simultaneously and begin and heat up, drop into sulfur-bearing again and be 6.613 tons of 32% troilite powders, squeeze into anolyte simultaneously to the effective volume liquid level, 91 ℃ of reactions 3 hours, this moment, solution contained manganese 38.21g/l, sulfur acid 3g/l, stop heating, about cooling tank liquor to 75～80 ℃.
2), add 10% ammoniacal liquor in the above-mentioned solution that reaches reaction end and neutralize, process temperature is controlled at 80 ℃, reaction is filtered 6.03 until pH value and is abandoned filter residue, must contain the rough manganese sulfate solution of manganese 38.27g/l, leaching yield reaches 92.3%.
3), above-mentioned rough manganese sulfate solution is squeezed in the next stage purification tank with the leaching vat equal volume, open stirring simultaneously, add ammonium sulfate to 130g/l, pH value fully after the dissolving, adds potassium permanganate 10kg 6.0, react after 1 hour, add Sodium Dimethyldithiocarbamate, till qualified except that nickel, filter then, filtrate is squeezed into the next stage purification tank, adds barium sulphide 120kg, and process temperature is controlled at 75～80 ℃, reaction times is 2 hours, filters to such an extent that slightly the step purifies manganese sulfate solution then.
4), above-mentioned coarse filtration being purified manganese sulfate solution squeezes in the next stage purification tank with the leaching vat equal volume, open stirring simultaneously, add XY-3 cleaner 28kg, process temperature is controlled at 75～80 ℃, reaction times is 2 hours, pH value is 6.0, filter then contain manganese 37.16g/l refining purification manganese sulfate solution use for electrowinning process.
The qualified refining purification manganese sulfate solution that present embodiment makes, the rate of recovery＞90%, electrolysis tech carries out electrolysis routinely, quality product is up to state standards, electrolysis output＞3kg/ veneer, power consumption≤7500kwh/ ton has realized that output, cost, the efficient of electrolytic manganese has surmounted the level that traditional employing manganous carbonate is produced electrolytic metal Mn.Wherein use various materials and all can arrive the market and buy, the XY-3 cleaner with the development of guest Davao, Guangxi scientific and technological development company for the most suitable.
Embodiment 2:
Present embodiment is substantially the same manner as Example 1, difference is, step 3) changes into: with step 2) the rough manganese sulfate solution of gained squeezes in the next stage purification tank with the leaching vat equal volume, open stirring simultaneously, add ammonium sulfate to 130g/l, pH value is 6.0, fully after the dissolving, add barium sulphide 120kg, process temperature is controlled at 75～80 ℃, reaction times is 2 hours, pH value filters the back and adds potassium permanganate 10kg 6.3, adds Sodium Dimethyldithiocarbamate after 1 hour, till qualified, filter to such an extent that slightly the step purifies manganese sulfate solution then except that nickel.
Embodiment 3:
Present embodiment is identical with embodiment 1 processing condition, but the system liquid of a kind of continuous leaching, purification, and the leaching vat that use are to be 180m by five useful volumes
3/ leaching vat are in series, and form three grades and leach continuously, and latter two purification tank is used for neutralization, and qualified neutralizer enters first purification tank after filtering continuously, and the purification tank that uses is to be 180m by seven useful volumes
3/ purification tank is in series, forming seven grades purifies continuously, wherein be provided with filtration facility between the 3rd purification tank and the 4th purification tank, also be provided with filtration facility between the 5th purification tank and the 6th purification tank, solution is standby after filtration after slipping out from last groove, be sent to electrowinning process.
Manganese oxide powder contains manganese 17%, and the troilite powder sulphur content is 32%, and anolyte contains manganese 12.6g/l, sulfur acid 32.68g/l, and concentration is 98% sulfuric acid, adds the dilution heat of sulfuric acid that water is mixed with 100g/l during use.
Processing step: with above-mentioned manganese oxide powder, troilite powder mixes by 1: 0.213 dry weight ratio, open the leaching vat agitator, squeeze into anolyte continuously toward first step leaching vat, heat up simultaneously and the above-mentioned breeze mixture of continuous input, the input speed of various materials satisfies manganese oxide powder, troilite powder, vitriolic weight ratio 1: 0.213: 0.36, feed liquid overflows from first step leaching vat and enters in the leaching vat of the second stage, from the leaching vat of the second stage, overflow again and enter in the third stage leaching vat, first, two, the temperature of three grades of leaching vat is 92 ℃, overflow from third stage leaching vat and last 3 hours from being dosed into feed liquid, when the feed liquid that overflows from third stage leaching vat has just entered as the 5th leaching vat of neutralizing well, the ammoniacal liquor of adding 10% carries out neutralization reaction continuously continuously in the 5th leaching vat, the control pH value is 6.0, the continuous continuously stirring of leaching vat at different levels, the 5th, need not heating in six grades of leaching vat, solution overflows to enter into from the 6th grade of leaching vat and enters pressure filter again behind the solution medial launder and filter, and filtered liquid continuously is driven in the first step purification tank; Add continuously in the first step purification tank and add ammonium sulfate, control its ammonium sulfate concentrations at 130g/l, with 60g/m
3The speed of manganese sulfate solution adds potassium permanganate continuously, and solution overflows from first step purification tank when entering second stage purification tank, with about 1.5kg/m
3The speed of manganese sulfate solution adds Sodium Dimethyldithiocarbamate continuously, and nickel is qualified to be as the criterion to remove, solution overflows to enter into from third stage purification tank and enters pressure filter again behind the solution medial launder and filter, filtered liquid continuously is driven in the fourth stage purification tank, simultaneously in the fourth stage purification tank with about 750g/m
3The speed of manganese sulfate solution adds barium sulphide continuously, solution overflows to enter into from the level V purification tank and enters pressure filter again behind the solution medial launder and filter, filtered liquid continuously is driven in the 6th grade of purification tank, simultaneously in the 6th grade of purification tank with about 17.5g/m
3The speed of manganese sulfate solution adds the XY-3 cleaner continuously, purification tanks at different levels are added 10% ammoniacal liquor according to circumstances, whole scavenging process control pH value is 6.0, the continuous continuously stirring of purification tanks at different levels need not heating, solution overflows to enter into from the 7th grade of purification tank and enters pressure filter again behind the solution medial launder and filter, and filtered liquid continuously is driven in the qualifying liquid storage tank and uses for electrowinning process.
The qualified refining purification manganese sulfate solution better quality that present embodiment makes, and continuous dosing and output, compare with the leaching, the purification process that are interrupted, the quantity of leaching vat and purification tank reduces about 50%, operator's quantity and working strength of workers can be and significantly reduce, and output is multiplied.
Claims (1)
1, a kind of liquid making technique of manganese oxide ore, leach the mixture of manganese oxide ore, sulfurous iron ore with sulfuric acid or sulphuric acid soln, the gained leaching liquid purifies with Sodium Dimethyldithiocarbamate, barium sulphide after neutralization is filtered again, and it is characterized in that: the liquid making technique of described manganese oxide ore may further comprise the steps successively:
1), manganese oxide powder, troilite powder, sulphuric acid soln or anolyte are put in the leaching vat, the process reaction temperature is controlled at 50～100 ℃, 1.5～6 hours time, manganese oxide powder, troilite powder, vitriolic weight ratio are 1: 0.09～0.40: 0.1～0.4, the reaction end sulfuric acid content is＜15g/l to obtain containing the leaching liquid of manganese 25～45g/l;
2), add neutralizing agent in the leaching liquid that obtains toward step 1) and neutralize, process temperature is controlled at 50～90 ℃, reaction is abandoned filter residue until pH value at 4.5～6.9 after-filtration, rough manganese sulfate solution;
3), get step 2) the rough manganese sulfate solution of gained, control its ammonium sulfate concentrations at 70～140g/l, add potassium permanganate, consumption is 10～100g/m
3Manganese sulfate solution after reacting completely, adds Sodium Dimethyldithiocarbamate, until remove nickel qualified till, add barium sulphide then or filter after in filtrate, add barium sulphide again, the barium sulphide consumption is 100g～2000g/m
3Manganese sulfate solution, process temperature is controlled at 30～80 ℃, reaction times is 0.5～3 hour, pH value is 4.5～6.9, filter to such an extent that slightly go on foot the purification manganese sulfate solution then, or get step 2) the rough manganese sulfate solution of gained, control its ammonium sulfate concentrations at 70～140g/l, add barium sulphide, the barium sulphide consumption is 100g～2000g/m
3Manganese sulfate solution, process temperature are controlled at 30～80 ℃, and the reaction times is 0.5～3 hour, and pH value filters the back and adds potassium permanganate 4.5～6.9, and consumption is 10～100g/m
3Manganese sulfate solution after reacting completely, adds Sodium Dimethyldithiocarbamate, till qualified except that nickel, filters to such an extent that slightly the step purifies manganese sulfate solution then;
4), get the step 3) gained and slightly go on foot the purification manganese sulfate solution, add the XY-3 cleaner, XY-3 cleaner consumption is 50g～400g/m
3The thick step purifies manganese sulfate solution, and process temperature is controlled at 30～80 ℃, and the reaction times is 0.5～3 hour, and pH value is 4.5～6.9, filter then refining purification manganese sulfate solution.
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| CN101845562A (en) * | 2010-06-22 | 2010-09-29 | 陈榜龙 | Improved device and method for producing electrolytic manganese metal by two-ore method |
| CN101880773A (en) * | 2010-06-13 | 2010-11-10 | 张安良 | Manufacturing process for producing synthetic reducing agent by using waste slag of electrolytic manganese and application of synthetic reducing agent |
| CN102220490A (en) * | 2011-05-06 | 2011-10-19 | 广西桂柳化工有限责任公司 | Production method of electrolytic manganese dioxide |
| CN102296323A (en) * | 2010-06-22 | 2011-12-28 | 陈榜龙 | Manufacturing system for producing electrolytic manganese metal by two-ore method |
| WO2012006935A1 (en) * | 2010-07-15 | 2012-01-19 | 广西有色金属集团汇元锰业有限公司 | Method for producing mercury-free alkaline-manganese type electrolyzed manganese dioxide |
| JP2013521206A (en) * | 2010-03-29 | 2013-06-10 | 貴州紅星発展股▲ふん▼有限公司 | Method for producing manganese sulfate monohydrate |
| CN103233119A (en) * | 2013-04-25 | 2013-08-07 | 国土资源部长沙矿产资源监督检测中心 | Process for producing manganese sulfate by treating two ores with acid |
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| CN107447111A (en) * | 2017-09-30 | 2017-12-08 | 柳州凯通新材料科技有限公司 | A kind of purification method of manganese sulfate electrolyte |
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- 2008-09-28 CN CN200810073819A patent/CN101684562A/en active Pending
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| CN101880773A (en) * | 2010-06-13 | 2010-11-10 | 张安良 | Manufacturing process for producing synthetic reducing agent by using waste slag of electrolytic manganese and application of synthetic reducing agent |
| CN101880773B (en) * | 2010-06-13 | 2013-01-30 | 张安良 | Manufacturing process for producing synthetic reducing agent by using waste slag of electrolytic manganese and application of synthetic reducing agent |
| CN102296323B (en) * | 2010-06-22 | 2014-11-05 | 陈榜龙 | Manufacturing system for producing electrolytic manganese metal by two-ore method |
| CN102296323A (en) * | 2010-06-22 | 2011-12-28 | 陈榜龙 | Manufacturing system for producing electrolytic manganese metal by two-ore method |
| WO2011160578A1 (en) * | 2010-06-22 | 2011-12-29 | Chen Banglong | Method for producing electrolytic manganese metal by using two ores and apparatus thereof |
| WO2011160575A1 (en) * | 2010-06-22 | 2011-12-29 | Chen Banglong | Manufacturing system for producing electrolytic manganese metal by two-mining method |
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| CN104862501A (en) * | 2015-05-07 | 2015-08-26 | 张安良 | Chemical clean beneficiation and accessory recycling process of lean manganese ore |
| CN107447111A (en) * | 2017-09-30 | 2017-12-08 | 柳州凯通新材料科技有限公司 | A kind of purification method of manganese sulfate electrolyte |
| CN107513625A (en) * | 2017-09-30 | 2017-12-26 | 柳州凯通新材料科技有限公司 | A kind of impurity-removing method of electrolytic manganese dioxide |
| CN114318417A (en) * | 2021-11-19 | 2022-04-12 | 赖厚党 | Method for producing electrolytic manganese by using low-grade manganese oxide three-ore method |
| CN114318417B (en) * | 2021-11-19 | 2024-05-03 | 赖厚党 | Method for producing electrolytic manganese by low-grade manganese oxide three-ore method |
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