CN101921914B - Iron removal process for copper cobalt ore leach liquor - Google Patents
Iron removal process for copper cobalt ore leach liquor Download PDFInfo
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- CN101921914B CN101921914B CN2010102848727A CN201010284872A CN101921914B CN 101921914 B CN101921914 B CN 101921914B CN 2010102848727 A CN2010102848727 A CN 2010102848727A CN 201010284872 A CN201010284872 A CN 201010284872A CN 101921914 B CN101921914 B CN 101921914B
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Abstract
The invention relates to an iron removal process for copper cobalt ore leach liquor, belonging to the cobalt wet smelting industry. At present, the goethite method and the precipitate neutralization iron removal method are combined to remove iron, although the total quantity of iron slag can be reduced, the total quantity of the iron slag is still great because the precipitate neutralization method with high pH value is used for removing iron at a later stage. The process is characterized by comprising the following steps of: firstly, oxidizing the liquor before iron removal to oxidize ferrous iron in the liquor into ferric iron; then, removing most of iron impurities in the oxidized liquor before iron removal by using the goethite method in an iron removal tank, and removing the rest iron and other metal impurities in the liquor by the precipitate neutralization iron removal method; and filter pressing the obtained ore pulp by using a filter press to obtain filter liquor as liquor after iron removal. Under the premise of ensuring the iron removal effect, the iron content in the iron slag is increased by changing the slag form of scrap iron slag, and thus, the total quantity of the iron slag is reduced.
Description
Technical field
The present invention relates to deferrization process, the deferrization process of copper-cobalt mine leachate in specifically a kind of cobalt hydrometallurgy industry.
Background technology
The hydrometallurgy of copper cobalt concentrate generally all is under sulfuric acid system, and valuable metals such as the Co in the mineral, Cu are leached in the solution, and solution is through purifying, and removes impurity such as wherein Fe, Mn, Mg, Al, Si, obtains comparatively purified cobalt sulfate solution; Because Fe belongs to the higher a kind of impurity of content in leach liquor, therefore, normally be equipped with independently production system in process of production it is handled.Contain a large amount of Fe in the copper-cobalt mine leachate, this part Fe is mainly with Fe
2+Form exist in solution, must before deironing, carry out oxide treatment to it, make it to become Fe
3+, just be easy to from solution, remove away.
The deironing of copper cobalt concentrate leach liquor has three kinds of methods usually: neutralization precipitation removes iron processes, goethite process and yellow modumite method.Adopt this three kinds of method deironing, can form the scum of different slag types, the quantity of slag is also different.The scum iron-holder that neutralization precipitation removes the iron processes generation is low, and the quantity of slag is maximum; Goethite process takes second place; The scum amount that yellow modumite method generates is minimum, and is comparatively harsh but this method requires technology controlling and process.Though it is big that neutralization precipitation removes the iron processes deironing quantity of slag, less demanding to technology controlling and process, and because the control of pH value is higher, the Fe in the solution can remove very thoroughly; Therefore, in industrial production, deironing normally uses goethite process or yellow modumite method to remove most iron earlier, with the neutralization precipitation method remaining a spot of Fe is removed again, so both can reach the few purpose of scum amount, can obtain clean cobalt liquid again.
Adopt two kinds of method interlock deironing; Will produce the scum of two kinds of forms, a kind of pyrrhosiderite slag (perhaps iron vitriol dreg of yellow sodium), a kind of is the neutralization precipitation scum; Earlier these two kinds of scums are mixed; Through the pressure filter press filtration, the clean cobalt liquid that obtains gets into next procedure then, and slag is then scrapped through behind the washery slag.Adopt two kinds of method interlock deironing,, also brought new problem though benefit is more; Neutralization precipitation removes iron processes because pH control is higher; Partial over-alkali makes other metal also precipitated, and includes valency metal Co, Cu; Caused scrap contain Co in the slag, Cu exceeds standard, and has reduced the yield of Co, Cu.Adopt two kinds of method interlock deironing,,, make the scum total amount still bigger because back segment has still used neutralization precipitation to remove the high pH deironing of iron processes though can reduce total quantity of slag of scum.Hope on the industrial production to take more excellent technological measure, reduce to the total amount of scum minimum.
In addition, in the oxide treatment to copper-cobalt mine leachate before deironing, Fe
2+Oxidation use oxidant hydrogen peroxide to inject tempering tank usually directly to mix with leach liquor, to reach Oxidation of Fe
2+Purpose because this method is in open container, to carry out, and discharges a large amount of heat in the reaction process, the partial oxygen air exhaustion that makes decomposing hydrogen dioxide solution discharge is prone in cell body, be discharged into the air, does not play abundant Oxidation of Fe
2+Effect, thereby cause the utilization ratio of ydrogen peroxide 50 lower.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective that above-mentioned prior art exists, and a kind of improved copper-cobalt mine leachate deferrization process is provided, and under the prerequisite that guarantees de-ferrous effect, in order to reduce Co, Cu content in the scum, improves the yield of valuable metal; Change the slag type of scrapping scum, improve the iron-holder in the scum, thereby reduce the total amount of scum.
For this reason; The present invention adopts following technical scheme: a kind of deferrization process of copper-cobalt mine leachate, and adopt goethite process and neutralization precipitation to remove the iron processes interlock, it is characterized in that earlier liquid before the deironing (being copper-cobalt mine leachate) being carried out oxide treatment; Making the oxidation of divalent in the solution is ferric iron; The pH value of solution is controlled at 0.8-1.5, and the liquid major part flows into behind the oxidation buffer jar in the iron removal trough before the deironing after the oxidation, and small portion flows into neutralization and removes in the scum pulp groove; Then, in iron removal trough, remove the most of iron contamination in the liquid before the deironing after the deoxidation with goethite process, the pH value of solution is controlled at 2.5-3.5, and the ore pulp that obtains use the pressure filter press filtration, directly scraps after the filter residue washing that obtains, and the filtrating inflow precipitates in the iron removal trough; In described deposition iron removal trough, add the alkaline carbonic acid sodium solution; Adopt neutralization precipitation to remove iron processes and remove remaining iron and other metallic impurity in the solution; The pH value of solution is controlled at 4.0-4.5, and the ore pulp that obtains is used the pressure filter press filtration, and the filter residue that obtains turns back in the oxidation buffer jar after the liquid dissolving is sized mixing before neutralization removes in the scum pulp groove with the deironing after the oxidation; And liquid gets into next removing in the ferrikinetics before the deironing after oxidation, and the filtrating that obtains is liquid after the deironing.The oxidation buffer groove is in order to guarantee Fe
2+Whole oxidations, if oxidation tank exports effusive solution Fe
2+Oxidation defective, can in dashpot, add into ydrogen peroxide 50, guarantee that its oxidation is qualified.
The present invention is with two kinds of slags (a kind of pyrrhosiderite slag that generates in the iron removal; A kind of neutralization removes scum) separately press filtration; Why the pyrrhosiderite slag is shifted to an earlier date press filtration; Be because the pyrrhosiderite slag is generation under the pH value about 3, not only most of impurity (Al, Si, Fe) can be from the system of opening a way out here, and valuable metal Co, Cu seldom precipitate; In addition, this pyrrhosiderite slag is because viscosity is little, and very easily washing is simultaneously because the slag iron content is high, so the total amount of slag is also few.
Neutralization remove scum because contain the valency metal Co, Cu is higher; So dissolve behind the scum again in the retrieval system with liquid before the deironing after the small portion oxidation; Get into next removing in the ferrikinetics, valuable metal Co, Cu are fully used, the consumption of liquid gets final product for the dissolving scum before the deironing; Because it is under the pH value about 4.5, to generate that neutralization removes scum; With neutralization reaction takes place during the liquid dissolving before the deironing after the oxidation of pH value about 1.0; Improved the pH value of liquid before the deironing that is used to get into after the subsequent processing oxidation, the consumption that can practice thrift auxiliary material sodium carbonate solution in the separation of iron in goethite form process.
Above-mentioned deferrization process; When liquid carried out oxide treatment before deironing, liquid mixed in line mixer with ydrogen peroxide 50 before the deironing, and mixed solution gets in two placed in-line airtight oxidation tanks and carries out oxidizing reaction; The flow pattern that solution goes out on adopting and advancing down requires before the deironing after the oxidation Fe in the liquid
2+Content is lower than 0.05g/L.Adopt line mixer will contain Fe earlier
2+Deironing before liquid and ydrogen peroxide 50 carry out pre-mixing, mixed solution gets in the oxidation tank and further carries out oxidizing reaction, the Fe in the assurance solution
2+Can all be oxidized to Fe
3+Airtight oxidation tank prevents that oxygen from escaping, and ydrogen peroxide 50 is fully used.
Above-mentioned deferrization process when using separation of iron in goethite form, adopts the pH value that adds alkaline carbonic acid sodium solution control solution.
Above-mentioned deferrization process, described oxidation buffer jar, iron removal trough and deposition iron removal trough are more than two, make that oxidizing reaction, deironing reaction carries out more fully, fully.
The beneficial effect that the present invention has: improve because the scum directly scrapped contains the Fe amount, reduced total quantity of slag of iron removal, also make it can be used as the raw material of other products, for the comprehensive utilization of scum lays the first stone; The scum that is used for directly scrapping is because viscosity is little, and very easily processing is conveniently scrapped in washing; Effectively reduce the valuable metal content in the slag, thereby improved the yield of valuable metal Co, Cu; Neutralization removes the scum retrieval system, has reduced the consumption of auxiliary material sodium carbonate solution, and liquid contains Fe and is lower than 0.02g/L after the deironing that the present invention obtains.
Below in conjunction with Figure of description and embodiment the present invention is described further.
Description of drawings
Fig. 1 is the used equipment flowsheet of deferrization process of the present invention.
Among the figure, 1, liquid before the deironing before the oxidation; 2, ydrogen peroxide 50; 3, line mixer; 4, airtight oxidation tank; 5, oxidation buffer groove; 6, iron removal trough; 7, separation of iron in goethite form dashpot; 8, pressure filter; 9, filter residue; 10, slag washing water; 11, pyrrhosiderite slag pulp groove; 12, filtrating; 13, send the slag operation to laundry; 14, deposition iron removal trough; 15, in and the deironing dashpot; 16, liquid before the deironing after the oxidation; 17, filter residue; 18, neutralization removes scum pulp groove; 19, filtrating; 20, turn back to the oxidation buffer groove; 21, sodium carbonate solution.
Embodiment
As shown in Figure 1, liquid 1 gets in the airtight oxidation tank 4 and proceeds oxidizing reaction with after ydrogen peroxide 50 2 mixes in line mixer 3 before the deironing before the oxidation.The ferrous solution that removes after the oxidation is divided into two portions; A part (70-90%, promptly most of) is to oxidation buffer groove 5, the existence of oxidation buffer groove; Can prolong oxidization time; If oxidation tank the inside oxidation is not thorough, can in oxidation buffer groove 5, adds ydrogen peroxide 50, thereby guarantee that the ferrous iron in the solution all is oxidized to ferric iron; Another part (10-30%, i.e. small portion) gets into neutralization and removes scum pulp groove 18.The solution entering iron removal trough 6 that comes out from oxidation buffer groove 5 carries out separation of iron in goethite form; After separation of iron in goethite form is accomplished; Slip gets into separation of iron in goethite form dashpot 7, and this slip is after pressure filter 8 press filtrations, and filter residue 9 is sent slag operation 13 after the pulp with slag washing water 10 in pyrrhosiderite slag pulp groove 11; Filtrate in 12 inflows and iron removal trough 14; Add the alkaline carbonic acid sodium solution, filtrating through in deironing after, during slip flows into deironing dashpot 15; And via pressure filter 8 press filtrations; Filtrating 19 gets into next processes, and liquid 17 removes in neutralization and turns back to oxidation buffer groove 5 after sizing mixing in the scum pulp groove 18 before the deironing after filter residue 16 and the small portion oxidation, and liquid gets into the next ferrikinetics that removes before the deironing after most of oxidation.
Each conditional request in the technology: the pH of liquid is about 1.0 before the deironing after (1) oxidation; (2) through behind the hydrogen peroxide oxidation, require Fe in the solution
2+Content is lower than 0.05g/L; (3) the pH value during separation of iron in goethite form is controlled at about 3.0, about temperature 85 degree; (4) the pH value of neutralisation deironing is controlled at about 4.5.
Claims (3)
1. the deferrization process of a copper-cobalt mine leachate; Adopt goethite process and neutralization precipitation to remove the iron processes interlock; It is characterized in that earlier liquid before the deironing being carried out oxide treatment, making the oxidation of divalent in the solution is ferric iron, and the pH value of solution is controlled at 0.8-1.5; The liquid major part flows into behind the oxidation buffer jar in the iron removal trough before the deironing after the oxidation, and small portion flows into neutralization and removes in the scum pulp groove; Then, in iron removal trough, remove the most of iron contamination in the liquid before the deironing after the deoxidation with goethite process, the pH value of solution is controlled at 2.5-3.5, and the ore pulp that obtains use the pressure filter press filtration, directly scraps after the filter residue washing that obtains, and the filtrating inflow precipitates in the iron removal trough; In described deposition iron removal trough, add the alkaline carbonic acid sodium solution; Adopt neutralization precipitation to remove iron processes and remove remaining iron and other metallic impurity in the solution; The pH value of solution is controlled at 4.0-4.5, and the ore pulp that obtains is used the pressure filter press filtration, and the filter residue that obtains turns back in the oxidation buffer jar after the liquid dissolving is sized mixing before neutralization removes in the scum pulp groove with the deironing after the oxidation; And liquid gets into next removing in the ferrikinetics before the deironing after oxidation, and the filtrating that obtains is liquid after the deironing;
When liquid carries out oxide treatment before deironing; Liquid mixes in line mixer with ydrogen peroxide 50 before the deironing; Mixed solution gets in two placed in-line airtight oxidation tanks and carries out oxidizing reaction, and the flow pattern that solution goes out on adopting and advancing down requires before the deironing after the oxidation Fe in the liquid
2+Content is lower than 0.05g/L.
2. deferrization process according to claim 1 when it is characterized in that using separation of iron in goethite form, adopts the pH value that adds alkaline carbonic acid sodium solution control solution.
3. deferrization process according to claim 1 is characterized in that described oxidation buffer jar, iron removal trough and deposition iron removal trough are more than two.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102848727A CN101921914B (en) | 2010-09-17 | 2010-09-17 | Iron removal process for copper cobalt ore leach liquor |
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| CN2010102848727A CN101921914B (en) | 2010-09-17 | 2010-09-17 | Iron removal process for copper cobalt ore leach liquor |
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| CN101921914B true CN101921914B (en) | 2012-07-25 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492841A (en) * | 2011-12-23 | 2012-06-13 | 天津市茂联科技有限公司 | Two-stage iron removal method for iron-containing solution |
| CN103014344A (en) * | 2012-12-31 | 2013-04-03 | 株洲冶炼集团股份有限公司 | Method for two-stage iron settlement in high-temperature peracid zinc leachate |
| CN103352122B (en) * | 2013-06-21 | 2015-11-25 | 刘国燕 | A kind of method of iron in efficient removal solution |
| CN103740931B (en) * | 2014-01-21 | 2015-11-18 | 江苏仁欣环保科技有限公司 | Containing the method for ferronickel mixing solutions goethite precipitation iron |
| CN104263943B (en) * | 2014-09-25 | 2017-02-15 | 池州西恩新材料科技有限公司 | Method for simultaneously separating chromium, iron and aluminum from acidic metal solution containing chromium, iron and aluminum |
| CN104498714B (en) * | 2014-12-22 | 2016-08-17 | 中南大学 | Ferrum, aluminum, calcium, the method for titana matter is removed from containing scandium solution separates |
| CN111286629A (en) * | 2018-12-07 | 2020-06-16 | 格林美（江苏）钴业股份有限公司 | Leaching process for cobalt-containing mineral aggregate |
| CN111304693A (en) * | 2018-12-12 | 2020-06-19 | 格林美（江苏）钴业股份有限公司 | Iron removal method for reducing accumulated iron ions in electrodeposition solution |
| CN110273070B (en) * | 2019-07-24 | 2022-06-17 | 中铝国际工程股份有限公司 | Iron removal method for copper sulfide concentrate oxygen pressure leaching solution |
| CN114317963A (en) * | 2021-12-27 | 2022-04-12 | 北方矿业有限责任公司 | Process method for efficiently removing iron by sectional catalytic oxidation |
| CN115725854A (en) * | 2022-11-16 | 2023-03-03 | 云南驰宏锌锗股份有限公司 | Magnetic fluid iron removal method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101086039A (en) * | 2007-06-22 | 2007-12-12 | 南通瑞翔新材料有限公司 | Copper cobalt alloy separation and recovery method |
| CN101117664A (en) * | 2007-09-05 | 2008-02-06 | 浙江华友钴镍材料有限公司 | Oxidation continuous deferrization process for copper cobalt liquor |
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- 2010-09-17 CN CN2010102848727A patent/CN101921914B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101086039A (en) * | 2007-06-22 | 2007-12-12 | 南通瑞翔新材料有限公司 | Copper cobalt alloy separation and recovery method |
| CN101117664A (en) * | 2007-09-05 | 2008-02-06 | 浙江华友钴镍材料有限公司 | Oxidation continuous deferrization process for copper cobalt liquor |
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