CN105861842A - Method for recovering lead from lead-containing material - Google Patents

Method for recovering lead from lead-containing material Download PDF

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Publication number
CN105861842A
CN105861842A CN201610438890.3A CN201610438890A CN105861842A CN 105861842 A CN105861842 A CN 105861842A CN 201610438890 A CN201610438890 A CN 201610438890A CN 105861842 A CN105861842 A CN 105861842A
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Prior art keywords
lead
containing material
solution
liquid
electrodeposition
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CN201610438890.3A
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CN105861842B (en
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王成彦
陈永强
邢鹏
马保中
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • 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
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for recovering lead from a lead-containing material, belonging to the technical field of hydrometallurgy. The method comprises the following steps: adding lead plaster or lead sulfate slag generated by zinc smelting into a ferrous chloride solution, leaching in a stirring mill so that the lead enters the solution, carrying out electrodeposition on the leach solution to obtain metallic lead, and returning the solution after lead electrodeposition to continue leaching the lead-bearing material. The technique has the characteristics of short process, fewer steps, low energy consumption cost and the like, and satisfies the environmental requirements for clean production.

Description

A kind of method reclaiming lead from lead-containing material
Technical field
The present invention relates to technical field of wet metallurgy, particularly relate to a kind of recovery from lead-containing material The method of lead.
Background technology
The exploitation of lead secondary resource at present have obtained increasing attention.Existing desulfurization The method of conversion+pyrometallurgical smelting is applied to the recovery of waste lead acid battery lead cream.Pyrometallurgy work It is high that skill processes lead plaster energy consumption cost, and can produce SO2, the atmosphere pollution such as volatility lead dust.
Another potential lead secondary resource, the sulphuric acid lead skim of zinc metallurgical process output, at present Also not obtaining effective exploitation, in this type of slag, Pb content is generally 20～50%.Lead in such slag Content is relatively low and lead is mainly lead sulfate, pyrometallurgic methods process same energy consumption high and Easily produce atmospheric pollution.By contrast, the method using hydrometallurgy processes sulphuric acid lead skim tool There are cleaning production, the advantage of valuable metal high efficiency extraction.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of side reclaiming lead from lead-containing material Method, it is achieved extracting directly obtains high-load from lead plaster or zinc metallurgical process output sulphuric acid lead skim Metallic lead.
The key step of the method is as follows:
(1) leach lead-containing material with solution of ferrous chloride for leaching agent, pass through after having leached Solid-liquor separation obtains leachate and leached mud；
(2) liquid after obtaining metallic lead and electrodeposition by electrodeposition in step (1) gained leachate；
(3), after liquid adding metallic iron reduction after the electrodeposition that step (2) obtains, gone back Former rear liquid, after reduction, liquid returns step (1) as leaching agent；When sulfate radical in liquid after reduction When ion concentration is more than 30g/L, by freezing and crystallizing make after reduction in liquid the sulfate radical of accumulation from Son precipitates with ferrous sulfate form partially crystallizable with ferrous ion, obtains ferrous sulfate crystal；
(4), after the ferrous sulfate dissolution of crystals that step (3) is obtained, add brium carbonate, enter Row barium salt removes lead, obtains pure ferrous sulfate product after recrystallization.
Wherein, the lead-containing material processed in step (1) is lead plaster or zinc metallurgical process output Sulphuric acid lead skim, wherein lead plaster contains Pb 60～75%, and sulphuric acid lead skim contains Pb 20～50%.
In step (1), leaching agent is solution of ferrous chloride, extraction temperature 20～90 DEG C, leaches Time 0.5～3h, solution of ferrous chloride concentration 100～450g/L, solution of ferrous chloride and leaded Liquid-solid ratio 20～40:1 in the mixed solution of material composition, leaching device therefor is Ball-stirring mill, leaching Go out process hydrochloric acid control solution pH at 0.5-1.5.
In step (2), the anode of electrolytic deposition process is insoluble anode, cathode-current density 100～300A/m2, electrodeposition temperature is room temperature.
In step (3), metallic iron is iron powder or iron plate, and the temperature of freezing and crystallizing is-10～0 DEG C.
Having the beneficial effect that of the technique scheme of the present invention:
(1) with pyrometallurgic methods ratio, the method energy consumption is low, meets the environmental protection that cleaning produces Requirement.
(2) the method technological process is succinct, easy and simple to handle, owing to ferrous chloride leaching agent can Recycling, put forward lead process and only consume a small amount of metallic iron, reagent consumption is few, low cost.Decapacitation Directly obtaining outside the metallic lead of high-load, the sulfate ion that accumulation enters in solution can be with ferrous iron Ion is crystallized with ferrous sulfate form by freezing and crystallizing, and the ferrum of reduction process consumption have also been obtained Regeneration.
Accompanying drawing explanation
Fig. 1 is the method process chart reclaiming lead from lead-containing material of the present invention.
Detailed description of the invention
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, below To be described in detail in conjunction with the drawings and the specific embodiments.
The present invention provides a kind of method reclaiming lead from lead-containing material, as it is shown in figure 1, for being somebody's turn to do The process chart of method, the method mainly include leaching, electrodeposition, reduction, freezing and crystallizing with And barium salt is except steps such as lead, is explained especially by embodiment.
Embodiment 1
Leaching: 1kg lead plaster (Pb 71.1%), leaching agent is 450g/L solution of ferrous chloride, Leach pH 1.0, extraction temperature 80 DEG C, extraction time 2h, liquid-solid ratio 35:1.Lead leaching rate Reach 98.1%.
Lead electrodeposition: take the above-mentioned leachate of 1.2L, at cathode area 0.01m2, cathode current is close Degree 150A/m2, electrodeposition under room temperature condition (25 DEG C), electrodeposition 5h, tank voltage 2.9V, Electricity lead 25.8g, electricity lead leaded 98%, electrolytic deposition process current efficiency 87.2%, power consumption 860.4kwh/t.
Reduction and freezing and crystallizing: use iron powder to make reducing agent, by ferric iron back in liquid after electrodeposition For ferrous iron.Under the conditions of-10～0 DEG C, by freezing and crystallizing in liquid after the electrodeposition of circulation, Formation ferrous sulfate crystallization precipitates, and controls the sulfate concentration in solution within 30g/L.
Barium salt removes lead: after the ferrous sulfate dissolution of crystals that will obtain, and adds brium carbonate, carries out barium Salt removes lead, obtains pure ferrous sulfate product after recrystallization.
Embodiment 2
Leach: 1kg sulphuric acid lead skim (Pb 45.7%), leaching agent is that 450g/L ferrous chloride is molten Liquid, leaches pH 1.0, extraction temperature 70 DEG C, extraction time 2h, liquid-solid ratio 29:1.Lead soaks Go out rate and reach 96.4%.
Lead electrodeposition: take the above-mentioned leachate of 1.2L, at cathode area 0.01m2, cathode current is close Degree 150A/m2, electrodeposition under room temperature condition (25 DEG C), electrodeposition 5h, tank voltage 2.85V, Electricity lead 25.9g, electricity lead leaded 98.2%, electrolytic deposition process current efficiency 87.8%, power consumption 839.7kwh/t。
Reduction and freezing and crystallizing: use iron powder to make reducing agent, by ferric iron back in liquid after electrodeposition For ferrous iron.Under the conditions of-10～0 DEG C, by freezing and crystallizing in liquid after the lead electrodeposition of circulation, Formation ferrous sulfate crystallization precipitates, and controls the sulfate concentration in solution within 30g/L with this.
Barium salt removes lead: after the ferrous sulfate dissolution of crystals that will obtain, and adds brium carbonate, carries out barium Salt removes lead, obtains pure ferrous sulfate product after recrystallization.
The above is the preferred embodiment of the present invention, it is noted that for the art Those of ordinary skill for, on the premise of without departing from principle of the present invention, it is also possible to do Going out some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (6)

1. the method reclaiming lead from lead-containing material, it is characterised in that: include following step Rapid:
(1) leach lead-containing material with solution of ferrous chloride for leaching agent, pass through after having leached Solid-liquor separation obtains leachate and leached mud；
(2) liquid after obtaining metallic lead and electrodeposition by electrodeposition in step (1) gained leachate；
(3), after liquid adding metallic iron reduction after the electrodeposition that step (2) obtains, gone back Former rear liquid, after reduction, liquid returns step (1) as leaching agent；When sulfate radical in liquid after reduction When ion concentration is more than 30g/L, by freezing and crystallizing make after reduction in liquid the sulfate radical of accumulation from Son precipitates with ferrous sulfate form partially crystallizable with ferrous ion, obtains ferrous sulfate crystal；
(4), after the ferrous sulfate dissolution of crystals that step (3) is obtained, add brium carbonate, enter Row barium salt removes lead, obtains pure ferrous sulfate product after recrystallization.
The method reclaiming lead from lead-containing material the most according to claim 1, its feature It is: the lead-containing material processed in described step (1) is lead plaster or zinc metallurgical process output Sulphuric acid lead skim, wherein lead plaster contains Pb 60～75%, and sulphuric acid lead skim contains Pb 20～50%.
The method reclaiming lead from lead-containing material the most according to claim 1, its feature It is: in described step (1), leaching agent is solution of ferrous chloride, extraction temperature 20～90 DEG C, Extraction time 0.5～3h, solution of ferrous chloride concentration 100～450g/L, solution of ferrous chloride and Liquid-solid ratio 20～40:1 in the mixed solution of lead-containing material composition, leaching device therefor is Ball-stirring mill, Leaching process with hydrochloric acid control solution pH at 0.5-1.5.
The method reclaiming lead from lead-containing material the most according to claim 1, its feature It is: in described step (2), the anode of electrolytic deposition process is insoluble anode, and cathode current is close Degree 100～300A/m2, electrodeposition temperature is room temperature.
The method reclaiming lead from lead-containing material the most according to claim 1, its feature It is: in described step (3), metallic iron is iron powder or iron plate.
The method reclaiming lead from lead-containing material the most according to claim 1, its feature It is: in described step (3), the temperature of freezing and crystallizing is-10～0 DEG C.
CN201610438890.3A 2016-06-17 2016-06-17 A kind of method that lead is reclaimed from lead-containing material Active CN105861842B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108754137A (en) * 2018-08-02 2018-11-06 桐乡市思远环保科技有限公司 The method that metallic lead is produced using solvent extraction electrodeposition process
CN110777394A (en) * 2019-10-24 2020-02-11 北京矿冶科技集团有限公司 Method for electrolyzing and recovering lead from lead-containing slag by using chlorination diaphragm

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101994007A (en) * 2009-08-28 2011-03-30 沈阳有色金属研究院 Method for removing sulfur from waste lead-acid storage battery gypsum mud by using magnesium chloride
CN102206750A (en) * 2011-05-04 2011-10-05 中南大学 Method for recovering lead from lead-containing material by matching leaching-electrowinning method
CN103194615A (en) * 2013-03-27 2013-07-10 云南祥云飞龙有色金属股份有限公司 Lead hydrometallurgical technology through utilizing lead sulfate
CN103757420A (en) * 2014-01-20 2014-04-30 北京矿冶研究总院 Method for recovering lead and silver from zinc leaching residues

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101994007A (en) * 2009-08-28 2011-03-30 沈阳有色金属研究院 Method for removing sulfur from waste lead-acid storage battery gypsum mud by using magnesium chloride
CN102206750A (en) * 2011-05-04 2011-10-05 中南大学 Method for recovering lead from lead-containing material by matching leaching-electrowinning method
CN103194615A (en) * 2013-03-27 2013-07-10 云南祥云飞龙有色金属股份有限公司 Lead hydrometallurgical technology through utilizing lead sulfate
CN103757420A (en) * 2014-01-20 2014-04-30 北京矿冶研究总院 Method for recovering lead and silver from zinc leaching residues

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108754137A (en) * 2018-08-02 2018-11-06 桐乡市思远环保科技有限公司 The method that metallic lead is produced using solvent extraction electrodeposition process
CN110777394A (en) * 2019-10-24 2020-02-11 北京矿冶科技集团有限公司 Method for electrolyzing and recovering lead from lead-containing slag by using chlorination diaphragm

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