CN106191463B - A kind of purification method of zinc hydrometallurgy leachate - Google Patents
A kind of purification method of zinc hydrometallurgy leachate Download PDFInfo
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- CN106191463B CN106191463B CN201610557321.0A CN201610557321A CN106191463B CN 106191463 B CN106191463 B CN 106191463B CN 201610557321 A CN201610557321 A CN 201610557321A CN 106191463 B CN106191463 B CN 106191463B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of purification methods of zinc hydrometallurgy leachate, especially suitable for high acidic oils Huang potassium (ammonium) Jarosite process except the solution of zinc sulfate or zinc oxide fumes sulphuric leachate after iron, the present invention is first with ferrous or supplement source of iron in oxidation solution to ensure the ferric concentration of solution, again by adding crystal seed lepidocrocite (γ FeOOH) slurry into reaction kettle, then it is slowly added to zinc sulfate leaching liquid to be cleaned, neutralizer is added simultaneously, and control pH value in reaction and temperature, make the ferric iron in solution, arsenic, germanium and fluorine plasma most or all enter precipitation, the precipitation slag of gained is easy to filter, washing.Present invention process process is simple, at low cost, not only may be implemented to process in zinc electrolyzing objectionable impurities（Iron, arsenic, fluorine and germanium etc.）Removal, while also realize germanium effective enrichment, be suitable for industrial applications.
Description
Technical field
The invention discloses a kind of purification methods of zinc hydrometallurgy leachate, belong to field of hydrometallurgy.
Background technology
Common method for removing iron has neutralization precipitation method, yellow potassium (ammonium) Jarosite process, goethite process (α-in solution purification
) and hematite process (Fe FeOOH2O3) etc., neutralization precipitation method is then to adjust pH precipitated irons oxidation of ferrous iron to ferric iron, this
The method quantity of slag is very big, is not easy to filter, and solution loss is big, and applicable solution is generally below 2g/L containing concentration of iron；Yellow potassium (ammonium) siderotil
Method is a kind of iron formation ihleite crystalloid precipitation made in zinc lixiviating solution and the zinc hot acid immersion liquid method for removing iron being removed, the world
The upper widely used such method for removing iron of zinc hydrometallurgy factory, technically comparative maturity, generated slag are easy to filter the method, but
Jarosite process generate needed for temperature it is high, reach 90 DEG C~95 DEG C, and except iron is not thorough, often can also remain 4 in solution~
The iron of 5g/L, produced ihleite slag have pollution to environment；Goethite process (alpha-feooh) is that iron side is commonly removed in hydrometallurgy
One of method, it is 90 DEG C~95 DEG C that goethite process operation, which needs temperature, and concentration of iron is required to be necessarily less than 1g/L；Hematite process
(Fe2O3) except iron rule needs to be more than 180 DEG C in temperature, it is operated under the high temperature and pressure system of 200~250kpa of oxygen partial pressure, iron
Removal rate is about 90%~95%.Above a variety of method for removing iron or there are filtration problems, or very harsh reaction condition is needed, all
It is not ideal method.
The processing method of arsenic removal comparison system is gone to have chemical precipitation method, Physical and microorganism in solution purification
Method.Widely applied chemical method mainly has neutralization precipitation method, flocculent precipitation, ferrite process, sulphide precipitation etc., only suitable
Processing for high concentration arsenic containing solution；Molysite arsenic removal is the common method of solution dearsenification, and molysite can water in meta-alkalescence solution
Solution generates ferric hydroxide colloid, which has huge absorption surface, can adsorb the ferric arsenate in waste water, and be co-precipitated,
But the ferric arsenate is a kind of amorphous precipitated object, and strainability is poor, and solubility is high, is unsuitable for storing up.Patent CN：
103911512A disclose arsenic removal in a kind of leachate from zinc abstraction, antimony method.Using zinc abstraction Weak-acid leaching liquid as raw material,
Using valuable constituents such as the heavy indium-hematite process arsenic removal of prereduction-neutralization, antimony technique purification synthetical recovery zinc, indium, iron.By low acid
Leachate is used as reducing agent using zinc concentrate, zinc sulfite, sulfur dioxide etc., and high price iron is made to be changed into low price iron, liquid after reduction
In high price iron (Fe3+) content is less than 2g/L, then is carried out in two sections using lime, lime stone, secondary zinc oxide, calcining, zinc oxide
Liquid pH value makes indium precipitation be enriched with for 4.0~5.4 after being restored with adjusting, and liquid reaches height using hematite process arsenic removal, antimony after heavy indium
Effect, the purpose of Cress solution.
Fluoride of the fluorine source of zinc hydrometallurgy industry in Zn dust, when leaching, enter solution, and fluorine ion can corrosion zinc
The cathode aluminum plate of electrolytic cell, makes zinc metal sheet remove, when the fluorine ion in solution is higher than 80mg/L, it is necessary to purify fluorine removal.Generally may be used
A small amount of milk of lime is added in leaching process, so that calcium hydroxide is formed insoluble calcirm-fluoride with fluorine ion and is that silica gel polymerize,
And be adsorbed on silica gel, make silica regeneration through water wash defluorinate, the fluoride removing rate of this method is only 26%~54%, and defluorination effect is not
It is good, and the introducing of lime will produce calcium sulfate scaling problem.Therefore general enterprises need in addition to increase a set of pyrogenic process pretreatment
Defluorinate system enters wet method system to reduce fluorine.A great problem in zinc hydrometallurgy industry fluorine removal, it would be highly desirable to it is a kind of efficiently, stablize,
Cheap treatment process.
Invention content
The purpose of the present invention is to provide a kind of technological processes, and simple, at low cost, safety and environmental protection zinc hydrometallurgy leaches
The method of liquid purification.
A kind of purification method of zinc hydrometallurgy leachate of the present invention, is as follows：
The first step：By original ferrous ion in Oxidation Leaching liquid, if ferrous ion and ferric iron in leachate
Ion concentration is not high, can be properly added ferric sulfate and adjust ferric ion concentration in solution, make ferric ion concentration range control
For system in 2~5g/L, ferric ion concentration is excessively high, and the loss of zinc can be caused excessive, too low, is unfavorable for subsequent precipitation；
In this step, by be added hydrogen peroxide or logical oxygen by the ferrous ions in leachate at ferric iron from
Son；
Due to zinc hydrometallurgy leachate generally all contain a small amount of ferric ion and ferrous ion, by oxidation or
Ferric iron is added, ensures ferric ion concentration, γ-FeOOH crystal seeds are introduced then at next step, makes ferric iron by adjusting pH
Precipitation forming core and is grown up on γ-FeOOH crystal seeds, finally precipitation rather than amorphous ferric hydroxide in the form of γ-FeOOH, no
Contamination precipitation removal is only realized, simultaneously because there are enough γ-FeOOH to go to adsorb some arsenic, germanium, fluorine plasma, is realized
Co-precipitation finally obtains sediment and is very easy to filtration washing.
Second step：The slurry for containing crystal seed-lepidocrocite (γ-FeOOH) is added in reaction kettle, opens stirring, and control
Temperature is to 25 DEG C~90 DEG C, and γ-FeOOH are used as crystal seed due to being, thus it is a small amount of, in use, first lepidocrocite water is beaten
Slurry is starched into, adsorption effect is more preferable；
Third walks：It is slowly added to the leachate for needing to purify into reaction kettle, while neutralizer is added, controlling reaction temperature
For 25 DEG C~90 DEG C and to maintain pH be 2.8~5.2；
4th step：10~30min of reaction is maintained after charging, is then separated by filtration, it can be according to by the filtrate of gained
Normal zinc wet method smelting process flow recycles zinc；
5th step：Gained filter residue can be used for conventional chlorinating distillation recovery germanium, dilute sulphur after being washed with dilution heat of sulfuric acid
Acid solution refers to the aqueous solution of sulfuric acid of the Solute mass fraction less than or equal to 70%.
The leachate is the neutral leachate, Weak-acid leaching liquid, jarosite process of zinc hydrometallurgy except molten after iron
The sulphuric leachate of liquid either zinc oxide fumes.
The crystal seed is lepidocrocite (γ-FeOOH), and iron ion (in γ-FeOOH) content is not less than in the slurry of addition
10g/L, in reaction process feed way be slow pair plus.
The neutralizer can be zinc calcine, zinc oxide, basic zinc carbonate, sodium carbonate, sodium hydroxide, ammonium hydroxide or carbon
Ammonium；Neutralizer is added in the form of solid powder, slurry or solution.
The precipitation process can generate in 25 DEG C~90 DEG C this extensive temperature ranges and be easy to washing, filtering
Precipitation slag.
The present invention, using slowly reaction pH is controlled to adduction, makes ferric ion in γ-by introducing γ-FeOOH crystal seeds
It forming core and grows up on FeOOH crystal seeds, finally precipitation rather than amorphous ferric hydroxide in the form of γ-FeOOH, while arsenic ion can
To precipitate or be adsorbed in the form of ferric arsenate；Arsenic ion, germanium ion and fluorine ion due to having preferable affinity with iron,
γ-FeOOH have powerful specific surface and adsorption capacity again, can be by Adsorption.Therefore, which can be realized simultaneously solution
Middle iron ion, arsenic ion, germanium ion and the removal of fluorine ion and the enriching and recovering of germanium.
The present invention is due to the adoption of the above technical scheme, very extensive at one with lepidocrocite (γ-FeOOH) for crystal seed
In temperature range, under the action of co-precipitation and absorption, realize that all or part of objectionable impurities ferric iron, arsenic, fluorine etc. is gone
It removes, while realizing the efficiently concentrating of germanium.
Compared with the method for existing zinc hydrometallurgy purification of leaching liquor, the present invention has the following advantages：
（1）Depth arsenic removal, germanium and ferric iron can be removed simultaneously, and realize effective enrichment of germanium.
（2）Relatively traditional deferrization process, to reaction temperature no requirement (NR), Applicable temperature range is wide, and low energy consumption.
（3）Technical process is simple, and no complicated special equipment requirement is readily produced application.
（4）Compared with traditional handicraft, the removal of fluorine is can be realized simultaneously, zinc electrolysis can be met, Funing tablet is wanted
It asks.
Present invention process process is simple, at low cost, not only may be implemented to the harmful impurity of process in zinc electrolyzing（Iron, arsenic,
Fluorine and germanium etc.）Removal, while also realizing effective enrichment of germanium, it is suitable for industrial applications.
Specific implementation mode
Embodiment 1：
It is 1.5 by 1L pH, 52mg/L containing germanium ion, arsenic ion 60mg/L, 85.6 g/L of zinc ion, fluorine ion
150 mg/L, ferric iron 0.2g/L, ferrous iron 2.2g/L zinc sulfate Weak-acid leaching liquid be added in beaker, add appropriate dioxygen
Water is all oxidized to ferric iron by ferrous, and supplements a small amount of ferric sulfate, and it is 5.0 g/L to make total iron concentration.
Lepidocrocite (γ-FeOOH) slurry of 30ml iron content 10g/L is added in a kettle as bottom liquid, opens stirring, control
25 DEG C of temperature processed, is slowly pumped into the Weak-acid leaching liquid through peroxidating, is at the same time also slowly added to the zinc calcine of 200 mesh, maintains
Solution system reacts pH=2.8.After the completion of waiting for zinc sulfate leaching liquid charging, continue to keep the 25 DEG C of reactions in reaction pH=3.5 and temperature
20 min, vacuum filtration, gained filter residue is after dilute sulfuric acid washing is dry, you can obtains rich germanium material.Iron in zinc sulfate leaching liquid
Ion, arsenic ion, germanium ion and fluorine ion total removal rate be respectively 99.8%, 99.3%, 99.4% and 65%, wherein fluorine is reacting
The residual in solution is about 45ppm afterwards, meets the 50ppm of zinc electrolysis requirement.
Embodiment 2：
It is 2.0 by 1L pH, 60mg/L containing germanium ion, arsenic ion 100mg/L, 73.6 g/L of zinc ion, fluorine ion 162
Mg/L, ferric ion 0.7g/L, ferrous ion 2.6g/L zinc oxide fumes sulphuric leachate be added in beaker, add
Appropriate hydrogen peroxide is all oxidized to ferric iron by ferrous.
Lepidocrocite (γ-FeOOH) slurry of 30ml iron content 20g/L is added in a kettle as bottom liquid, opens stirring, control
Temperature 45 C processed is slowly pumped into the zinc oxide fumes sulphuric leachate through peroxidating, is at the same time also slowly added to ammonium bicarbonate（Carbonic acid
Hydrogen ammonium）Saturated solution maintains solution system to react pH=4.0.After the completion of waiting for zinc sulfate leaching liquid charging, continue to keep reaction pH
Stop reaction with 25 min of temperature, vacuum filtration, gained filter residue is after dilute sulfuric acid washing is dry, you can obtains rich germanium material.Oxygen
Change iron ion in Zn dust sulphuric leachate, arsenic ion, germanium ion and fluorine ion total removal rate be respectively 99.9%, 99.5%,
99.5% and 73%, wherein residual of the fluorine after the reaction in solution is about 42ppm, meets the 50ppm of zinc electrolysis requirement.
Embodiment 3：
It is 3.5 by 1L pH, 10mg/L containing germanium ion, arsenic ion 22mg/L, 62.5 g/L of zinc ion, fluorine ion 82
Mg/L, ferrous ion 0.6g/L zinc sulfate solution be added in beaker, while being passed through oxygen, all aoxidized ferrous
For ferric iron, and adding ferric sulfate makes solution total concentration reach 3g/L.
Lepidocrocite (γ-FeOOH) slurry of 30ml iron content 15g/L is added in a kettle as bottom liquid, opens stirring, control
85 DEG C of temperature processed, is slowly pumped into the zinc sulfate leaching liquid through peroxidating, is at the same time also slowly added to sodium hydroxide solution, maintains
Solution system reacts pH=4.8.After the completion of waiting for zinc sulfate leaching liquid charging, continue that reaction pH and 20 min of temperature is kept to stop instead
It answers, is filtered by vacuum, gained filter residue is after dilute sulfuric acid washing is dry, you can obtains rich germanium material.Zinc oxide fumes sulphuric leachate
Middle iron ion, arsenic ion, germanium ion and fluorine ion total removal rate be respectively 99.9%, 99.9%, 99.5% and 68%, wherein fluorine exists
Residual after reaction in solution is about 27ppm, meets the 50ppm of zinc electrolysis requirement.
Embodiment 4：
It is 2.0 by 1L pH, 30mg/L containing germanium ion, arsenic ion 10mg/L, 110 g/L of zinc ion, fluorine ion 105
Mg/L, ferric ion 3.5g/L, the zinc calcine high acidic oils liquid of ferrous ion 0.6g/L are upper after jarosite process removes iron
Clear liquid（Referred to as：Heavy alum supernatant）It is added in beaker, adds appropriate hydrogen peroxide, all ferric iron is oxidized to by ferrous.
Lepidocrocite (γ-FeOOH) slurry of 30ml iron content 10g/L is added in a kettle as bottom liquid, opens stirring, control
90 DEG C of temperature processed, is slowly pumped into the zinc oxide fumes sulphuric leachate through peroxidating, and it is solid to be at the same time also slowly added to sodium carbonate
Body maintains solution system to react pH=4.0.After the completion of waiting for zinc sulfate leaching liquid charging, continue to keep reaction pH and 10 min of temperature
Stop reaction, be filtered by vacuum using heat preservation, gained filter residue is after dilute sulfuric acid washing is dry, you can obtains rich germanium material.On heavy alum
Iron ion in clear liquid, arsenic ion, germanium ion and fluorine ion total removal rate be respectively 99.9%, 99.2%, 99.7% and 66.7%,
Residual of the middle fluorine ion after the reaction in solution is about 35ppm, meets the 50ppm of zinc electrolysis requirement.
Claims (7)
1. a kind of purification method of zinc hydrometallurgy leachate, which is characterized in that the purification method includes the following steps：
The first step：It is ferric ion by the ferrous ions in leachate, then adjusts ferric ion concentration in leachate
For 2~5g/L；
Second step：Crystal seed lepidocrocite slurry is added in reaction kettle, is stirred, and control temperature to 25 DEG C~90 DEG C；
Third walks：After the first step treated leachate is added into reaction kettle, neutralizer is added, it is 2.8 to maintain reaction pH
~5.2, reaction temperature is 25 DEG C~90 DEG C；
4th step：The reaction was continued after charging 10~30min, is then separated by filtration, the filter residue safe handling that will be obtained.
2. a kind of purification method of zinc hydrometallurgy leachate according to claim 1, it is characterised in that：Add in the first step
It is ferric ion to add hydrogen peroxide or be passed through oxygen by ferrous ions.
3. a kind of purification method of zinc hydrometallurgy leachate according to claim 1, it is characterised in that：Add in the first step
Add ferrum sulfuricum oxydatum solutum that ferric ion concentration in leachate is made to be 2~5g/L.
4. a kind of purification method of zinc hydrometallurgy leachate according to claim 1, it is characterised in that：The zinc is wet
It is that the neutral leachate, Weak-acid leaching liquid, jarosite process of zinc hydrometallurgy remove solution or oxygen after iron that method, which smelts leachate,
Change the sulphuric leachate of Zn dust.
5. a kind of purification method of zinc hydrometallurgy leachate according to claim 1, it is characterised in that：It is brilliant in second step
Iron content is not less than 10g/L in kind lepidocrocite slurry.
6. a kind of purification method of zinc hydrometallurgy leachate according to claim 1, it is characterised in that：Institute in third step
The neutralizer stated is one or more of zinc calcine, zinc oxide, basic zinc carbonate, sodium carbonate, sodium hydroxide, ammonium hydroxide or ammonium bicarbonate.
7. a kind of purification method of zinc hydrometallurgy leachate according to claim 1, it is characterised in that：Mistake in 4th step
It filters isolated filter residue and washs afterchlorinate distillation recovery germanium with dilution heat of sulfuric acid.
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| CN106868304A (en) * | 2016-12-27 | 2017-06-20 | 河南豫光锌业有限公司 | A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum |
| CN107058740A (en) * | 2017-02-10 | 2017-08-18 | 河南理工大学 | A kind of titanium white method for treating waste liquid |
| CN107233884B (en) * | 2017-06-05 | 2020-06-30 | 云南驰宏锌锗股份有限公司 | Ferromagnetic catalyst for catalyzing hydrolysis and precipitation of trivalent iron, and preparation method and application thereof |
| CN108034818B (en) * | 2017-11-29 | 2019-09-13 | 中国科学院过程工程研究所 | Method for synchronously removing impurity elements in manganese sulfate leaching solution through in-situ neutralization and synergistic adsorption |
| CN108467942B (en) * | 2018-02-13 | 2020-01-10 | 武汉科技大学 | Method for selectively leaching zinc, lead, gallium and germanium from zinc replacement slag |
| CN109970105B (en) * | 2019-04-24 | 2021-04-16 | 西南科技大学 | Method for cleanly recovering iron in zinc hydrometallurgy process |
| CN110255623B (en) * | 2019-07-24 | 2021-12-14 | 中国科学院过程工程研究所 | Iron and arsenic separation method, separation device and application thereof |
| CN111172408B (en) * | 2020-01-20 | 2022-06-10 | 昆明瀚创科技有限公司 | Control method of zinc sulfate solution continuous deep purification nickel-cobalt-germanium removing equipment |
| CN114703379B (en) * | 2022-02-21 | 2023-09-22 | 云锡文山锌铟冶炼有限公司 | Method for deeply purifying neutral leaching solution of zinc hydrometallurgy |
| CN115652104B (en) * | 2022-11-01 | 2023-09-12 | 中南大学 | Lead-free jarosite crystal, jarosite slag, preparation method and application |
| CN116623002B (en) * | 2023-05-04 | 2024-02-23 | 西部矿业股份有限公司 | Method for removing magnesium ions in zinc hydrometallurgy based on solution crystallization method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS52106317A (en) * | 1976-03-05 | 1977-09-06 | Akita Seiren Kk | Method of separating deposits of hydrated iron from slime of zinc leaching |
| CN100357192C (en) * | 2006-01-16 | 2007-12-26 | 深圳市危险废物处理站 | Deferrization method of iron-containing liquor |
| RU2382091C1 (en) * | 2008-11-17 | 2010-02-20 | Государственное образовательное учреждение высшего профессионального образования Томский политехнический университет | Reprocessing method of zinc concentrate |
| CN101629246B (en) * | 2009-08-03 | 2011-03-30 | 杨志杰 | Zinc smelting process by neutralization and hydrolysis iron removal method |
| CN101713031B (en) * | 2009-10-26 | 2011-05-18 | 德阳市南邡有色金属有限公司 | Method for removing impurities by oxidation in process of zinc hydrometallurgy |
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