CN106756008B - The method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions leach lead in concentrate of lead sulfide ore - Google Patents
The method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions leach lead in concentrate of lead sulfide ore Download PDFInfo
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- CN106756008B CN106756008B CN201710098319.6A CN201710098319A CN106756008B CN 106756008 B CN106756008 B CN 106756008B CN 201710098319 A CN201710098319 A CN 201710098319A CN 106756008 B CN106756008 B CN 106756008B
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
- C22B3/165—Leaching with acyclic or carbocyclic agents of a single type with organic acids
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
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- 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
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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
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Abstract
The invention discloses a kind of methods that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions leach lead in concentrate of lead sulfide ore, this method is to mix sulfonic acid solutions in a kettle with concentrate of lead sulfide ore, surfactant, oxidation catalyst is done using iron ion, pass through neutral alumina leaching under normal pressure and leach this two sections of counterflow leaching process with acidic oxidation, realizes the selectively leaching of lead；And the sulphur in concentrate is oxidized to elementary sulfur, remains in slag.Neutral leachate obtains metallic lead and useless electric effusion by electrodeposition；Useless electric effusion matches electric effusion as acidic leaching next time or with new liquid；Acid leaching solution enters next time neutral leach.This method not only realizes the high efficiency extraction of lead, and realizes recycling for leachate and electric effusion, and no waste liquid generates, and meets environmentally protective requirement.
Description
Technical field
The present invention relates to a kind of method for extracting lead from concentrate of lead sulfide ore by Whote-wet method, more particularly to a kind of sulfonic acid is molten
The method that two sections of adverse current atmospheric pressure oxidations of liquid leach lead in concentrate of lead sulfide ore, belongs to non-ferrous metallurgy field.
Background technology
Sulfonic acid solutions are stabilized in nature, not oxidizable and reduction.There are many purposes, are medical and pesticide materials,
It can be used as dehydrating agent, paint solidification accelerating agent, fibre finish, obtained extensive use as electric brush plating liquor solvent in recent years.Gold
Belong to metilsulfate to widely apply in field of electrochemical deposition, wherein including with the relevant application of surface finishing industry:In tin, lead
And fluoboric acid and borofluoride are substituted in Terne Electroplating；Wire and steel bar are tin plating；The Metal Finishing of silver, copper, nickel and palladium；
Nickel, tin, lead, tin-lead and cadmium coater are stripped from copper and its alloy, zinc and its alloy surface using dipping and spray coating method.
The lead of 80% or more the country is that pyrogenic process produces from concentrate of lead sulfide ore at present.Traditional pyrometallurgical smelting of lead is using sintering
By burning-blast furnace reduction process, big, low concentration SO that there are energy consumptions2Exhaust emission environment, is forbidden to use by country.State at present
The present lead metallurgical method of inside and outside use has bottom blowing molten pool melting (such as QSL methods, Shuikoushan method), Flash Smelting Furnace melting (such as Ji Fusai
Special method), the methods of top-blown submergence smelting process (such as Ausmelt method, ISA methods), these smelting processes, reaction temperature is 1100
DEG C or more, high energy consumption, lead steam is high, pollutes environment.
Currently, the method that research wet method extracts lead from concentrate of lead sulfide ore both at home and abroad has：①FeCl3Oxidizing process：PbS+2FeCl3
=PbCl2+2FeCl2+S0, various dissoluble lead-Chloro complexes are formed under higher temperature, are passed through and alkali metal chloride is added is increased
Cl-Total concentration, the lead in solution can be made mainly with PbCl4 2-Form exist, then crystallisation by cooling goes out PbCl2, re-dry, most
The electrolytic metal lead in low-temperature molten salt system afterwards, anode generate chlorine, and chlorine, which returns, to be leached, but it there are problems to be：Hydrochloric acid is easy
Volatilization, equipment seriously corroded；Molten-salt electrolysis high temperature chlorine be not easy to collect and molten-salt electrolysis lead in lead chloride production is contacted with air
Raw lead oxide, hinders the progress of electrolysis.Also there are the research of ozone-hydrogen peroxide-ferric trichloride co-oxidation extraction, reaction side
Formula is as follows：
PbS+4H2O2+ 2NaCl=PbCl2+Na2SO4+4H2O
3PbS+4O3+ 6NaCl=3PbCl2+3Na2SO4
PbS+2NaCl+8FeCl3+4H2O=PbCl2+Na2SO4+8FeCl2+8HCl
8FeCl2+H2O2+3H2O+O3+ 8HCl=8FeCl3+8H2O
PbCl2+ 2Cl-=[PbCl4]2-
2. galena-pyrolusite two-ores method：It is born in oxidisability oxidation galena using manganese dioxide in pyrolusite
Sulfidion, to leach lead, manganese element simultaneously.Reaction equation is as follows：
PbS+MnO2+ 4HCl=PbCl2+MnCl2+S0+2H2O
PbCl2+2Cl-=[PbCl4]2-
3. the Oxidation Leaching in fluosilicic acid medium：Oxidant used has oxygen, H2O2、Fe2(SiF6)3, their reaction is:
2PbS+O2+2H2SiF6=2PbSiF6+2S0+2H2O
PbS+H2O2+H2SiF6=PbSiF6+S0+2H2O
PbS+Fe2(SiF6)3=PbSiF6+S0+2FeSiF6
Using oxygen, H2O2Lead is leached, it can be with electrodeposition lead after purified；Fe2(SiF6)3For oxidant, need to use conjunctiva
Electrodeposition, cathode obtain lead, and anode regenerates Fe2(SiF6)3.But leaching agent fluoride is unstable, easy decomposition generates hydrogen fluoride gas,
It is harmful, cause operating environment poor.
Invention content
For existing pyrometallurgical smelting of lead and wet underwater welding lead method that there are environmental pollutions is serious, leaching agent corrosivity is big,
The problems such as operating environment is poor, the purpose of the present invention is be to propose environmentally protective, the efficient Whote-wet method of one kind from concentrate of lead sulfide ore
The method of middle extraction lead.
In order to achieve the above technical purposes, the present invention provides a kind of two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions to leach vulcanization
The method of lead in lead concentrate, this approach includes the following steps：
1) after mixing concentrate of lead sulfide ore, surfactant with leaching agent containing sulfonic acid, under normal pressure, oxygen is blasted into system
Gas, carries out neutral leaching, and solid-liquor separation obtains neutral leachate and neutral leaching residue；
2) the neutral leachate described in is made into lead electric effusion with useless electric effusion and carries out electro-deposition lead, obtains metal stereotype and gives up
Electric effusion；
3) after the neutral leaching residue described in is mixed with acid lixiviant, under normal pressure, oxygen is blasted into system, carry out acid
Property leach, solid-liquor separation obtains acid leaching solution and acidic leaching residue；The acid lixiviant is generated useless by electro-deposition lead
Electric effusion supplements to be obtained within the scope of its free sulfonic concentration to 0.3~2.5mol/L；
4) acid leaching solution enters neutral leach next time as leaching agent containing sulfonic acid and uses, the acidic leaching residue
Carry out recycling elementary sulfur and valuable metal.
Preferred scheme, the leaching agent containing sulfonic acid include pyrovinic acid and/or ethylsulfonic acid.
Preferred scheme, the neutrality leaching condition are：The liquid-solid ratio of leaching agent containing sulfonic acid and concentrate of lead sulfide ore is 3mL/g
~15mL/g, the quality of surfactant are the 0.05~0.5% of concentrate of lead sulfide ore quality, and reaction temperature is 85~100 DEG C, is stirred
It is 100~800 revs/min to mix speed, and the reaction time is 15~30h, and reaction end pH value is 5.0 or more.
More preferably scheme, the surfactant include at least one in ligninsulfonate, o-phenylenediamine, m-phenylene diamine (MPD)
Kind.
The condition of preferred scheme, the acidic leaching is：The liquid-solid ratio of neutral leaching residue and acid lixiviant is 3mL/g
~15mL/g, extraction temperature are 90~105 DEG C, and mixing speed is 200~1000 revs/min, and extraction time is 15~30h, is leached
Terminal point control system acidity is 0.1~0.8mol/L.
The condition of preferred scheme, the electro-deposition lead is：Current density is 80~400A/m2, electric effusion temperature 30
~65 DEG C.
More preferably scheme, during electro-deposition lead, using graphite cake, ti-supported lead dioxide electric net or titanium-based platinum guaze as anode
Plate, using Lead initiated plate electrode, titanium plate or stainless steel plate as cathode plate；The cathode plate periphery is 1~3 centimetre longer than the anode plate.
The method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions provided by the invention leach lead in concentrate of lead sulfide ore includes following
Step (Fig. 1 is shown in technological process)：
1) by concentrate of lead sulfide ore, surfactant (such as ligninsulfonate, o-phenylenediamine, m-phenylene diamine (MPD)) and last time acid
Property leach acid immersion liquid (it includes sulfonic acid) mixing, in open reactive tank, to stirring slurry below blast oxygen into
Row reaction, finally makes leachate at weakly acidic pH；And make ferrous ions therein at ferric iron, during ferric iron precipitation enters
Property leached mud in, then carry out solid-liquor separation obtain neutral leachate and neutral leaching residue.Neutral leaching condition is：Acid immersion liquid
Liquid-solid ratio with concentrate of lead sulfide ore is 3mL/g~15mL/g, and surfactant is concentrate of lead sulfide ore amount 0.05~0.5%, reaction
Temperature be 85~100 DEG C, mixing speed be 100~800 revs/min, the reaction time be 15~30h, reaction end pH value 5.0 with
On.There is key reaction in neutral leaching process：
2PbS+4RSO3H+O2=2Pb (RSO3)2+S°+2H2O
PbS+2RSO3H+2Fe3+=2Pb (RSO3)2+S°+2Fe2++H2O
4Fe2++O2+6H2O=4FeOOH+8H+
R is CH in reaction equation3、C2H5。
2) above-mentioned neutral leachate and useless electric effusion are made into the sulfonic acid solutions of certain lead concentration (lead concentration, which meets electrodeposition, to be wanted
Ask), electro-deposition obtains metal stereotype and useless electric effusion.Electro-deposition lead process：Current density is 80~400A/m2, electrodeposition
30~65 DEG C of liquid temperature.During electrodeposition lead, using graphite cake, ti-supported lead dioxide electric net or titanium-based platinum guaze as anode plate, begun with lead
Pole piece, titanium plate or stainless steel plate are cathode plate；The cathode plate periphery is 1~3 centimetre longer than the anode plate.Electro-deposition lead process
Key reaction has：
4Pb(RSO3)2+2H2O=4Pb+O2+4RSO3H
3) (the useless electric effusion adjusts its free sulfonic concentration to above-mentioned neutral leaching residue using sulfonic acid solutions with useless electric effusion
Within the scope of 0.3~2.5mol/L) mixing, neutrality, which leaches the iron oxide to precipitate and reacts to dissolve with sulfonic acid, enters solution,
Blast oxygen to stirring slurry bottom in open reactive tank, make the neutral sulphur for leaching unreacted vulcanized lead be oxidized to elementary sulfur into
Enter to acidic leaching residue, and lead dissolving enters solution.After solid-liquor separation, acid leaching solution and acidic leaching residue are obtained.Acidity leaching
Going out condition is：Extraction temperature is 90~105 DEG C, and mixing speed is 200~1000 revs/min, 15~30h of extraction time, is leached eventually
The acidity for selecting leachate, which is 0.1-0.8mol/L acidic leaching process key reactions, to be had：
FeOOH+3H+=Fe3++2H2O
PbS+2RSO3H+2Fe3+=2Pb (RSO3)2+S0+2Fe2++H2O
2PbS+4RSO3H+O2=2Pb (RSO3)2+S0+2H2O
4) above-mentioned acid leaching solution enters neutral leach next time and uses, and leached mud recycles elementary sulfur and valuable gold
Belong to.
Compared with the prior art, the advantageous effect that technical scheme of the present invention is brought：With pyrometallurgical smelting of lead, lead, lead oxide are eliminated
Steam volatilizees, and does not have SO2The discharge of flue gas, avoids environmental pollution；Lead is refined with existing wet method, leaching agent toxicity is low, rotten
Corrosion is small, good operational environment.In addition, the present invention realizes the complete alternation between electric effusion, leachate, no waste liquid generates, and meets
Environmental requirement.In conclusion the method for the present invention is a kind of method of green, clean extraction lead.
Description of the drawings
【Fig. 1】For the process flow chart of the present invention.
Specific implementation mode
Further illustrated with reference to example, following instance be intended to further illustrate the present invention and not to invention into one
Step limits.
Embodiment 1
Experiment concentrate of lead sulfide ore chemical composition such as table 1 used.
The chemical composition of 1 concentrate of lead sulfide ore of table
| Element | Pb | S | Fe | Ag |
| Ingredient/% | 48.71 | 17.32 | 7.76 | 0.0057 |
Concentrate of lead sulfide ore 400g (its chemical composition such as table 1) is taken, acid leaching solution 2000mL is added, chemical composition is：
Pb2+120g/L, iron ion total concentration are 0.15mol/L, and dissociate a concentration of 0.3mol/L of pyrovinic acid；And the wooden sulphurs of 0.5g are added
Sour calcium blasts oxygen, mixing speed 350r/ to agitating paddle bottom while stirring in the cylinder reactor according of diameter 10cm
Min reacts 20h at 95 DEG C of temperature, until solution ph 5.3, after iron ion total concentration is less than 5mg/L, Separation of Neutral leachate
With neutral leaching residue.
The useless electric effusions of 2000mL are added in neutral leaching residue, and useless electric effusion ingredient is：Pb2+35g/L, pyrovinic acid concentration of dissociating
For 1.2mol/L oxygen, mixing speed are blasted to agitating paddle bottom while stirring in the cylinder reactor according of diameter 10cm
300r/min reacts 22h at 95 DEG C of temperature.Reaction is completed to be separated by filtration acid leaching solution and acidic leaching residue.
The electric effusion 3000mL that gives up is added in neutral leachate, and useless electric effusion ingredient is：Pb2+35g/L, pyrovinic acid concentration of dissociating
For 1.2mol/L, it is made into the solution of lead content 70g/L.Using ti-supported lead dioxide electric net as anode, lead flake is cathode, pole span 4cm, electricity
Accumulated temperature degree is 40 DEG C, current density 250A/m2Under the conditions of, electrodeposition 20h, current efficiency reaches 99.86%.
Acidic leaching residue dry weight 210.5g, lead-in-dreg 1.21%, analysis result show the leaching rate of lead up to 98.69%, and
Noble silver, gold fully enter in leached mud.
Comparative example 1
Concentrate of lead sulfide ore 400g (its chemical composition such as table 1) is taken, acid leaching solution 2000mL is added, chemical composition is：
Pb2+120g/L, iron ion total concentration are 0.15mol/L, and dissociate a concentration of 0.3mol/L of pyrovinic acid；And the wooden sulphurs of 0.5g are added
Sour calcium blasts oxygen, mixing speed 350r/ from agitating paddle bottom while stirring in the cylinder reactor according of diameter 10cm
Min reacts 6h at 95 DEG C of temperature, until solution ph 5.3, after iron ion total concentration is less than 5mg/L, Separation of Neutral leachate with
Neutral leaching residue.
The useless electric effusions of 2000mL are added in neutral leaching residue, and useless electric effusion ingredient is：Pb2+35g/L, pyrovinic acid concentration of dissociating
For 1.2mol/L oxygen, mixing speed are blasted from agitating paddle bottom while stirring in the cylinder reactor according of diameter 10cm
300r/min reacts 6h at 95 DEG C of temperature.Reaction is completed to be separated by filtration acid leaching solution and acidic leaching residue.
Acidic leaching residue dry weight 320.8g, lead-in-dreg 28.67%, analysis result show the leaching rate only 52.91% of lead, and
Part lead is remained in vulcanized lead in slag, and noble silver, gold fully enter in leached mud.
Claims (5)
1. the method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions leach lead in concentrate of lead sulfide ore, it is characterised in that：Including following step
Suddenly：
1) after mixing concentrate of lead sulfide ore, surfactant with leaching agent containing sulfonic acid, under normal pressure, oxygen is blasted into system,
Neutral leaching is carried out, solid-liquor separation obtains neutral leachate and neutral leaching residue；Neutral leaching condition is：Leaching agent containing sulfonic acid
Be 3mL/g~15mL/g with the liquid-solid ratio of concentrate of lead sulfide ore, the quality of surfactant be concentrate of lead sulfide ore quality 0.05~
0.5%, reaction temperature is 85~100 DEG C, and mixing speed is 100~800 revs/min, and the reaction time is 15~30h, reaction end
PH value is 5.0 or more；
2) the neutral leachate described in is made into lead electric effusion with useless electric effusion and carries out electro-deposition lead, obtains metal stereotype and useless electrodeposition
Liquid；
3) after the neutral leaching residue described in is mixed with acid lixiviant, under normal pressure, oxygen is blasted into system, carry out acid leaching
Go out, solid-liquor separation obtains acid leaching solution and acidic leaching residue；The useless electrodeposition that the acid lixiviant is generated by electro-deposition lead
Liquid supplements to be obtained within the scope of its free sulfonic concentration to 0.3~2.5mol/L；The condition of the acidic leaching is：Neutral leaching residue
Liquid-solid ratio with acid lixiviant is 3mL/g~15mL/g, and extraction temperature is 90~105 DEG C, and mixing speed is 200~1000
Rev/min, extraction time is 15~30h, and leaching terminal point control system acidity is 0.1~0.8mol/L；
4) acid leaching solution enters neutral leach next time as leaching agent containing sulfonic acid and uses, and the acidic leaching residue carries out
Recycle elementary sulfur and valuable metal.
2. the method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions according to claim 1 leach lead in concentrate of lead sulfide ore,
It is characterized in that：The leaching agent containing sulfonic acid includes pyrovinic acid and/or ethylsulfonic acid.
3. the method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions according to claim 1 leach lead in concentrate of lead sulfide ore,
It is characterized in that：The surfactant includes at least one of ligninsulfonate, o-phenylenediamine, m-phenylene diamine (MPD).
4. the method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions according to claim 1 leach lead in concentrate of lead sulfide ore,
It is characterized in that：The condition of the electro-deposition lead is：Current density is 80~400A/m2, 30~65 DEG C of electric effusion temperature.
5. the method that two sections of adverse current atmospheric pressure oxidations of sulfonic acid solutions according to claim 1 or 4 leach lead in concentrate of lead sulfide ore,
It is characterized in that：During electro-deposition lead, using graphite cake, ti-supported lead dioxide electric net or titanium-based platinum guaze as anode plate, with lead beginning pole
Piece, titanium plate or stainless steel plate are cathode plate；The cathode plate periphery is 1~3 centimetre longer than the anode plate.
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| CN110343873B (en) * | 2019-08-02 | 2022-01-07 | 中南大学 | Normal-pressure oxygen-enriched leaching method for bismuth sulfide concentrate in methanesulfonic acid system |
| CN110629043B (en) * | 2019-09-04 | 2021-11-19 | 长沙有色冶金设计研究院有限公司 | Bismuth extraction method based on phase transformation of bismuth sulfide ore |
| CN111659530B (en) * | 2020-06-16 | 2021-03-23 | 昆明理工大学 | Method for dressing, smelting, recovering and separating continuous growth type copper-lead-zinc sulfide ore |
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| CN1083118A (en) * | 1992-08-16 | 1994-03-02 | 个旧市矿产加工总厂 | With the technology of silicofluoric acid from the concentrate of lead sulfide ore leaching lead |
| CN100393896C (en) * | 2007-01-22 | 2008-06-11 | 中国科学院过程工程研究所 | New method for soaking out enriched ores of high indium, high iron, and high sulfur zinc |
| CN101760623A (en) * | 2009-12-28 | 2010-06-30 | 长沙理工大学 | Wet leaching method of galena |
| CN103540743B (en) * | 2012-07-13 | 2015-06-03 | 张超 | Hydrometallurgical method of metal sulfides |
| US9322105B2 (en) * | 2012-11-13 | 2016-04-26 | The University Of British Columbia | Recovering lead from a lead material including lead sulfide |
| US9322104B2 (en) * | 2012-11-13 | 2016-04-26 | The University Of British Columbia | Recovering lead from a mixed oxidized material |
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