CN106191463A - A kind of purification method of zinc hydrometallurgy leachate - Google Patents

A kind of purification method of zinc hydrometallurgy leachate Download PDF

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Publication number
CN106191463A
CN106191463A CN201610557321.0A CN201610557321A CN106191463A CN 106191463 A CN106191463 A CN 106191463A CN 201610557321 A CN201610557321 A CN 201610557321A CN 106191463 A CN106191463 A CN 106191463A
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zinc
leachate
purification
solution
zinc hydrometallurgy
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CN201610557321.0A
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Chinese (zh)
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CN106191463B (en
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周兆安
张银亮
刘小文
姚标
毛谙章
米永红
李钧
冯凡让
郑晓凤
马千里
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深圳市危险废物处理站有限公司
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/20Obtaining zinc otherwise than by distilling
    • C22B19/26Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses the purification method of a kind of zinc hydrometallurgy leachate, it is particularly well-suited to high acidic oils Huang potassium (ammonium) Jarosite process except the solution of zinc sulfate after ferrum or zinc oxide fumes sulphuric leachate, the present invention first with oxidation solution in ferrous or supplementary source of iron to ensure the ferric concentration of solution, again by adding crystal seed lepidocrocite (γ FeOOH) slurry in reactor, then it is slowly added to treat the zinc sulfate leaching liquid of remove impurity, it is simultaneously introduced nertralizer, and control pH value in reaction and temperature, make the ferric iron in solution, arsenic, germanium and most or all entrance precipitations of fluorine plasma, the precipitation slag of gained is prone to filter, washing.Present invention process process is simple, low cost, is possible not only to achieve the removal to process in zinc electrolyzing objectionable impurities (ferrum, arsenic, fluorine and germanium etc.), also realizes effective enrichment of germanium, it is adaptable to industrial applications simultaneously.

Description

A kind of purification method of zinc hydrometallurgy leachate
Technical field
The invention discloses the purification method of a kind of zinc hydrometallurgy leachate, belong to field of hydrometallurgy.
Background technology
Method for removing iron conventional in solution purification have neutralization precipitation method, yellow potassium (ammonium) Jarosite process, goethite process (α- And hematite process (Fe FeOOH)2O3) etc., neutralization precipitation method is oxidation of ferrous iron to ferric iron, then regulation pH precipitated iron, this The method quantity of slag is very big, is difficult to filter, and solution loss is big, and its solution being suitable for is generally below 2g/L containing concentration of iron;Yellow potassium (ammonium) siderotil Method is that a kind of ferrum made in zinc lixiviating solution forms ihleite crystalloid precipitation and the zinc hot acid immersion method for removing iron that is removed, the world Widely used this kind of method for removing iron of upper zinc hydrometallurgy factory, the method comparative maturity technically, produced slag is prone to filter, but Temperature needed for jarosite process generates is high, reaches 90 DEG C~95 DEG C, and except ferrum is thorough, often solution also can remain 4~ The ferrum of 5g/L, the ihleite slag produced has pollution to environment;Goethite process (alpha-feooh) is conventional except ferrum side in hydrometallurgy One of method, it is 90 DEG C~95 DEG C that goethite process operation needs temperature, and requires that concentration of iron is necessarily less than 1g/L;Hematite process (Fe2O3) except iron rule needs in temperature more than 180 DEG C, operate under the High Temperature High Pressure system of oxygen partial pressure 200~250kpa, ferrum Clearance is about 90%~95%.The most multiple method for removing iron or there is filtration problem, or need the harshest reaction condition, all It it not ideal method.
The processing method removing arsenic removal comparison system in solution purification has chemical precipitation method, Physical and microorganism Method.Wide variety of chemical method mainly has neutralization precipitation method, flocculent precipitation, ferrite process, sulphide precipitation etc., the suitableeest Process for high concentration arsenic containing solution;Iron salt arsenic removal is the common method of solution dearsenization, and iron salt can water in meta-alkalescence solution Solving and generate ferric hydroxide colloid, this colloid has huge absorption surface, can adsorb the ferric arsenate in waste water, and be co-precipitated, But this ferric arsenate is a kind of amorphous precipitated thing, and strainability is poor, dissolubility is high, is unsuitable for storing up.Patent CN: 103911512A discloses a kind of arsenic removal from zinc abstraction leachate, the method for antimony.With zinc abstraction Weak-acid leaching liquid as raw material, Heavy indium-hematite process the arsenic removal of prereduction-neutralization, antimony technique is used to purify the valuable constituents such as synthetical recovery zinc, indium, ferrum.By low acid Leachate uses zinc concentrate, zinc sulfite, sulfur dioxide etc. as reducing agent, makes high price ferrum be changed into ferrum, liquid after reduction at a low price In high price ferrum (Fe3+) content is less than 2g/L, then use Calx, limestone, secondary zinc oxide, calcining, zinc oxide to carry out in two sections Being 4.0~5.4 to make indium precipitation enrichment with liquid pH value after regulation reduction, after heavy indium, liquid uses hematite process arsenic removal, antimony, reaches high Effect, the purpose of Cress solution.
The fluorine source of zinc hydrometallurgy industry fluoride in Zn dust, enters solution during leaching, fluorion can corrosion zinc The cathode aluminum plate of electrolysis bath, makes zinc metal sheet peel off, when the fluorion in solution is higher than 80mg/L, it is necessary to purify fluorine removal.Typically may be used In leaching process, add a small amount of lime cream, make calcium hydroxide form insoluble calcium fluoride with fluorion and be that silica gel is polymerized, And adsorb on silica gel, and making silica regeneration through water wash defluorinate, the fluoride removing rate of the method is only 26%~54%, and defluorination effect is not Good, and the introducing of Calx can produce calcium sulfate scaling problem.Therefore general enterprises needs additionally 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 a kind of efficiently, stable, Cheap process technique.
Summary of the invention
It is an object of the invention to provide a kind of technological process zinc hydrometallurgy simple, low cost, safety and environmental protection to leach The method that liquid purifies.
The purification method of a kind of zinc hydrometallurgy leachate of the present invention, specifically comprises the following steps that
The first step: by ferrous ion original in Oxidation Leaching liquid, if ferrous ion and ferric ion in leachate Content is the highest, can be properly added ferric ion concentration in iron sulfate regulation solution, make ferric ion concentration scope control 2 ~5g/L, ferric ion concentration is too high, and the loss that can cause zinc is excessive, the lowest, is unfavorable for precipitation below;
In this step, by adding hydrogen peroxide or logical oxygen, the ferrous ions in leachate is become ferric ion;
Owing to zinc hydrometallurgy leachate the most all contains a small amount of ferric ion and ferrous ion, by oxidation or interpolation Ferric iron, it is ensured that ferric ion concentration, introduces γ-FeOOH crystal seed then at next step, makes ferric iron sink by regulation pH Form sediment, forming core growing up on γ-FeOOH crystal seed, finally precipitate with γ-FeOOH form, rather than amorphous ferric hydroxide, not only Achieve contamination precipitation to remove, simultaneously because there are enough γ-FeOOH to go to adsorb some arsenic, germanium, fluorine plasma, it is achieved altogether Precipitation, finally gives precipitate and is very easy to filtration washing.
Second step: join in reactor by the slurry containing crystal seed-lepidocrocite (γ-FeOOH), opens stirring, and controls Temperature is to 25 DEG C~90 DEG C, owing to being γ-FeOOH as crystal seed, so a small amount of, during use, first lepidocrocite water is beaten Slurry form slurry, adsorption effect is more preferable;
3rd step: be slowly added to the leachate needing to purify in reactor, be simultaneously introduced nertralizer, controlling reaction temperature is 25 DEG C~90 DEG C and to maintain pH be 2.8~5.2;
4th step: charging maintains reaction 10~30min after terminating, and then filters separation, can be according to normally by the filtrate of gained Zinc wet method smelting process flow process reclaim zinc;
5th step: can be used for conventional chlorinating Distillation recovery germanium after the washing of gained filtering residue dilution heat of sulfuric acid, described dilute sulfuric acid is molten Liquid refers to that Solute mass fraction is less than or equal to the sulfur aqueous acid of 70%.
Described leachate is molten except after ferrum of the neutral leachate of zinc hydrometallurgy, Weak-acid leaching liquid, jarosite process Liquid or the sulphuric leachate of zinc oxide fumes.
Described crystal seed is lepidocrocite (γ-FeOOH), and in the slurry of addition, iron ion (in γ-FeOOH) content is not less than 10g/L, in course of reaction, feed way is slowly to adding.
Described nertralizer can be zinc calcine, zinc oxide, basic zinc carbonate, sodium carbonate, sodium hydroxide, ammonia or carbon Ammonium;Nertralizer uses the form of pressed powder, slurry or solution to add.
Described precipitation process can this be widely in temperature range at 25 DEG C~90 DEG C, produces and is prone to washing, filters Precipitation slag.
The present invention, by introducing γ-FeOOH crystal seed, uses and adduction slowly controls reaction pH, make ferric ion γ- Forming core growing up on FeOOH crystal seed, finally precipitates with γ-FeOOH form, rather than amorphous ferric hydroxide, arsenic ion can simultaneously Precipitate or adsorbed with the form with ferric arsenate;Arsenic ion, germanium ion and fluorion owing to having preferable affinity with ferrum, γ-FeOOH has again powerful specific surface and absorbability, can be adsorbed removing.Therefore, this technique can realize solution simultaneously The removal of middle iron ion, arsenic ion, germanium ion and fluorion, and the enriching and recovering of germanium.
Due to the fact that employing technique scheme, with lepidocrocite (γ-FeOOH) as crystal seed, at one widely In temperature range, under the effect by co-precipitation and absorption, it is achieved completely or partially going of objectionable impurities ferric iron, arsenic, fluorine etc. Remove, realize the efficiently concentrating of germanium simultaneously.
Compared with the method for existing zinc hydrometallurgy purification of leaching liquor, the invention have the advantages that
(1) degree of depth can remove arsenic removal, germanium and ferric iron simultaneously, and achieve effective enrichment of germanium.
(2) relatively conventional deferrization process, it is to reaction temperature no requirement (NR), and Applicable temperature scope is wide, and energy consumption is low.
(3) technical process is simple, without complicated special equipment requirement, it is easy to production application.
(4) compared with traditional handicraft, the removal of fluorine can be realized so that it is zinc electrolysis can be met Funing tablet is wanted simultaneously Ask.
Present invention process process is simple, low cost, be possible not only to achieve to the harmful impurity of process in zinc electrolyzing (ferrum, arsenic, Fluorine and germanium etc.) remove, also realize effective enrichment of germanium, it is adaptable to industrial applications simultaneously.
Detailed description of the invention
Embodiment 1:
It is 1.5 by 1L pH, containing germanium ion 52mg/L, arsenic ion 60mg/L, zinc ion 85.6 g/L, fluorion 150 Mg/L, ferric iron 0.2g/L, the zinc sulfate Weak-acid leaching liquid of ferrous 2.2g/L join in beaker, add appropriate hydrogen peroxide, will Ferrous iron is all oxidized to ferric iron, and supplements a small amount of iron sulfate, and making total iron concentration is 5.0 g/L.
Add lepidocrocite (γ-FeOOH) slurry of 30ml iron content 10g/L in a kettle. as end liquid, unlatching stirring, control Temperature processed 25 DEG C, slowly pumps into through snperoxiaized Weak-acid leaching liquid, is the most also slowly added to the zinc calcine of 200 mesh, maintains Solution system reaction pH=2.8.After zinc sulfate leaching liquid has fed, continue to keep reaction pH=3.5 and temperature 25 DEG C reaction 20 min, vacuum filtration, gained filtering residue is dried through dilute sulfuric acid washing, i.e. available rich germanium material.Ferrum in zinc sulfate leaching liquid The total removal rate of ion, arsenic ion, germanium ion and fluorion is respectively 99.8%, 99.3%, 99.4% and 65%, and wherein fluorine is in reaction Residual in rear solution is about 45ppm, meets the 50ppm of zinc electrolysis requirement.
Embodiment 2:
It is 2.0 by 1L pH, containing germanium ion 60mg/L, arsenic ion 100mg/L, zinc ion 73.6 g/L, fluorion 162 mg/ L, ferric ion 0.7g/L, the zinc oxide fumes sulphuric leachate of ferrous ion 2.6g/L join in beaker, add appropriate Hydrogen peroxide, is all oxidized to ferric iron by ferrous iron.
Add lepidocrocite (γ-FeOOH) slurry of 30ml iron content 20g/L in a kettle. as end liquid, unlatching stirring, control Temperature 45 C processed, slowly pumps into through snperoxiaized zinc oxide fumes sulphuric leachate, is the most also slowly added to carbon ammonium (carbonic acid Hydrogen ammonium) saturated solution, maintain solution system reaction pH=4.0.After zinc sulfate leaching liquid has fed, continue to keep reaction pH With temperature 25 min stopped reaction, vacuum filtration, gained filtering residue is dried through dilute sulfuric acid washing, i.e. available rich germanium material.Oxygen Change the total removal rate of iron ion in Zn dust sulphuric leachate, arsenic ion, germanium ion and fluorion be respectively 99.9%, 99.5%, 99.5% and 73%, wherein the residual in fluorine solution after the reaction is about 42ppm, meets the 50ppm of zinc electrolysis requirement.
Embodiment 3:
Be 3.5 by 1L pH, containing germanium ion 10mg/L, arsenic ion 22mg/L, zinc ion 62.5 g/L, fluorion 82 mg/L, The zinc sulfate solution of ferrous ion 0.6g/L joins in beaker, is passed through oxygen simultaneously, and ferrous iron is all oxidized to three Valency ferrum, and add iron sulfate and make overall solution concentration reach 3g/L.
Add lepidocrocite (γ-FeOOH) slurry of 30ml iron content 15g/L in a kettle. as end liquid, unlatching stirring, control Temperature processed 85 DEG C, slowly pumps into through snperoxiaized zinc sulfate leaching liquid, is the most also slowly added to sodium hydroxide solution, maintains Solution system reaction pH=4.8.After zinc sulfate leaching liquid has fed, continue to keep reaction pH and temperature 20 min to stop anti- Should, vacuum filtration, gained filtering residue is dried through dilute sulfuric acid washing, i.e. available rich germanium material.Zinc oxide fumes sulphuric leachate The total removal rate of middle iron ion, arsenic ion, germanium ion and fluorion is respectively 99.9%, 99.9%, 99.5% and 68%, and wherein fluorine exists After reaction, the residual in solution is about 27ppm, meets the 50ppm of zinc electrolysis requirement.
Embodiment 4:
Be 2.0 by 1L pH, containing germanium ion 30mg/L, arsenic ion 10mg/L, zinc ion 110 g/L, fluorion 105 mg/L, Ferric ion 3.5g/L, ferrous ion 0.6g/L zinc calcine high acidic oils liquid through jarosite process except the supernatant after ferrum (being called for short: heavy vitriol supernatant) joins in beaker, adds appropriate hydrogen peroxide, ferrous iron is all oxidized to ferric iron.
Add lepidocrocite (γ-FeOOH) slurry of 30ml iron content 10g/L in a kettle. as end liquid, unlatching stirring, control Temperature processed 90 DEG C, slowly pumps into through snperoxiaized zinc oxide fumes sulphuric leachate, is the most also slowly added to sodium carbonate solid Body, maintains solution system reaction pH=4.0.After zinc sulfate leaching liquid has fed, continue to keep reaction pH and temperature 10 min Stopped reaction, uses insulation vacuum filtration, and gained filtering residue is dried through dilute sulfuric acid washing, i.e. available rich germanium material.On heavy vitriol In clear liquid, the total removal rate of iron ion, arsenic ion, germanium ion and fluorion is respectively 99.9%, 99.2%, 99.7% and 66.7%, its Residual in middle fluorion solution after the reaction is about 35ppm, meets the 50ppm of zinc electrolysis requirement.

Claims (9)

1. the purification method of a zinc hydrometallurgy leachate, it is characterised in that described purification method comprises the steps:
The first step: be ferric ion by the ferrous ions in leachate, then regulate ferric ion concentration in leachate It is 2~5g/L;
Second step: crystal seed lepidocrocite slurry is joined in reactor, stirring, and control temperature to 25 DEG C~90 DEG C;
3rd step: after adding the leachate after the first step processes in reactor, add nertralizer, maintaining reaction pH is 2.8 ~5.2, reaction temperature is 25 DEG C~90 DEG C;
4th step: charging continues reaction 10~30min after terminating, and then filters separation, the filtering residue safe handling that will obtain.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: the first step adds Add hydrogen peroxide or to be passed through oxygen by ferrous ions be ferric ion.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: the first step adds Adding ferrum sulfuricum oxydatum solutum makes ferric ion concentration in leachate be 2~5g/L.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: described zinc is wet It is that the neutral leachate of zinc hydrometallurgy, Weak-acid leaching liquid, jarosite process are except the solution after ferrum or oxygen that method smelts leachate Change the sulphuric leachate of Zn dust.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: brilliant in second step In planting lepidocrocite slurry, iron content is not less than 10g/L.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: in the 3rd step The addition manner of mediating recipe is for adding.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: institute in the 3rd step The nertralizer stated is more than one in zinc calcine, zinc oxide, basic zinc carbonate, sodium carbonate, sodium hydroxide, ammonia or carbon ammonium.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: mistake in the 4th step The filtering residue of filter isolated washs afterchlorinate Distillation recovery germanium with dilution heat of sulfuric acid.
The purification method of a kind of zinc hydrometallurgy leachate the most according to claim 1, it is characterised in that: mistake in the 4th step The filtrate of filter isolated continues to reclaim zinc according to zinc wet method smelting process.
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Cited By (7)

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Publication number Priority date Publication date Assignee Title
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
CN107233884A (en) * 2017-06-05 2017-10-10 云南驰宏锌锗股份有限公司 It is a kind of to be used to be catalyzed ferromagnetism catalyst of ferric iron hydrolytic precipitation and its preparation method and application
CN108034818A (en) * 2017-11-29 2018-05-15 中国科学院过程工程研究所 A kind of method of impurity element in original position neutralization-synergistic sorption simultaneous removing manganese sulfate leachate
CN108467942A (en) * 2018-02-13 2018-08-31 武汉科技大学 A method of Selectively leaching zinc, lead, gallium and germanium from zinc replacement slag
CN109970105A (en) * 2019-04-24 2019-07-05 西南科技大学 A kind of method of cleaning recycling iron in Zinc hydrometallurgy process
CN110255623A (en) * 2019-07-24 2019-09-20 中国科学院过程工程研究所 Iron arsenic separation method, separator and its application

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RU2382091C1 (en) * 2008-11-17 2010-02-20 Государственное образовательное учреждение высшего профессионального образования Томский политехнический университет Reprocessing method of zinc concentrate
CN101713031A (en) * 2009-10-26 2010-05-26 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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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN107233884A (en) * 2017-06-05 2017-10-10 云南驰宏锌锗股份有限公司 It is a kind of to be used to be catalyzed ferromagnetism catalyst of ferric iron hydrolytic precipitation and its preparation method and application
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
CN108034818A (en) * 2017-11-29 2018-05-15 中国科学院过程工程研究所 A kind of method of impurity element in original position neutralization-synergistic sorption simultaneous removing manganese sulfate leachate
CN108034818B (en) * 2017-11-29 2019-09-13 中国科学院过程工程研究所 It is a kind of original position neutralization-synergistic sorption simultaneous removing manganese sulfate leachate in impurity element method
CN108467942A (en) * 2018-02-13 2018-08-31 武汉科技大学 A method of Selectively leaching zinc, lead, gallium and germanium from zinc replacement slag
CN109970105A (en) * 2019-04-24 2019-07-05 西南科技大学 A kind of method of cleaning recycling iron in Zinc hydrometallurgy process
CN110255623A (en) * 2019-07-24 2019-09-20 中国科学院过程工程研究所 Iron arsenic separation method, separator and its application

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