CN106834679B - The method that lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions - Google Patents
The method that lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions Download PDFInfo
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- CN106834679B CN106834679B CN201710097359.9A CN201710097359A CN106834679B CN 106834679 B CN106834679 B CN 106834679B CN 201710097359 A CN201710097359 A CN 201710097359A CN 106834679 B CN106834679 B CN 106834679B
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- lead
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- sulfonic acid
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/06—Preparation of sulfur; Purification from non-gaseous sulfides or materials containing such sulfides, e.g. 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- 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
Abstract
The invention discloses a kind of methods that lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions, this method is reacted in autoclave after mixing sulfonic acid solutions with concentrate of lead sulfide ore, surfactant, oxidation catalyst is done using iron ion, by neutral oxygen leaching and this two sections of counterflow leaching process of acid oxygen leaching, the selectively leaching of lead is realized；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 enters acidic leaching next time or for preparing new electric effusion.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 lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of liquid, belongs to non-ferrous metallurgy field.
Background technology
Sulfonic acid solutions are stabilized in nature, not oxidizable and reduction.Sulfonic acid is that medicine and pesticide are former there are many purposes
Material, can be used as dehydrating agent, paint solidification accelerating agent, fibre finish, has obtained extensive use as electric brush plating liquor solvent in recent years.
Metal metilsulfate is widely applied in field of electrochemical deposition, wherein including with the relevant application of surface finishing industry:Tin,
Fluoboric acid and borofluoride are substituted in lead and Terne Electroplating；Wire and steel bar are tin plating；The metal essence of silver, copper, nickel and palladium
Decorations；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 are high, pollute 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
Electrolytic metal lead and chlorine in low-temperature molten salt system afterwards, chlorine, which returns, to be leached, but it there are problems to be：Hydrochloric acid is volatile, rotten
Lose equipment, high temperature chlorine be not easy to collect and molten-salt electrolysis lead in lead chloride contact generation lead oxide with air, hinder to be electrolysed
It carries out.Also there are the research of ozone-hydrogen peroxide-ferric trichloride co-oxidation extraction, reaction equation 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+S+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 it is a kind of it is environmentally protective, efficiently by Whote-wet method from vulcanized lead
The method that lead is extracted in concentrate.
In order to achieve the above technical purposes, the present invention provides a kind of two sections of adverse current pressure oxidations of sulfonic acid solutions to leach vulcanization
The method of lead in lead concentrate, this approach includes the following steps：
1) it after mixing concentrate of lead sulfide ore, surfactant with leaching agent containing sulfonic acid, is transferred in autoclave, leads into system
Enter oxygen, carry out neutral leaching, 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) it after the neutral leaching residue described in is mixed with acid lixiviant, is transferred in autoclave, oxygen is passed through into system, into
Row acidic leaching after solid-liquor separation, obtains acid leaching solution and acidic leaching residue；The acid lixiviant is produced by electro-deposition lead
Raw useless 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 noble metal.
Preferred scheme, the leaching agent containing sulfonic acid include pyrovinic acid and/or ethylsulfonic acid.
Preferred scheme, neutral leaching condition are：The liquid-solid ratio of leaching agent containing sulfonic acid and concentrate of lead sulfide ore be 3mL/g~
15mL/g, surfactant qualities are the 0.05~0.5% of concentrate of lead sulfide ore quality, and reaction temperature is 105~170 DEG C, stirring
Speed is 100~800 revs/min, and it is 0.5~3h that oxygen, which presses 0.2~1.5MPa, reaction time, and reaction end pH value is 5.0 or more.
More preferably scheme, surfactant used 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 110~170 DEG C, and mixing speed is 200~800 revs/min, and oxygen presses 0.2~1.5MPa, when leaching
Between be 0.5~3.0h, leachings terminal point control system acidity be 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℃。
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 lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions provided by the invention includes following
Step (attached drawing 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, pressurised oxygen is carried out in the autoclave of certain temperature and oxygen pressure
Change and leach, finally makes leachate at weakly acidic pH；And making ferrous ions therein at trivalent, precipitation enters neutral leaching residue
In, it then carries out solid-liquor separation and obtains neutral leachate and neutral leaching residue.Neutral leaching condition is：The liquid of leaching agent and concentrate
Gu than being 3mL/g~15mL/g, surfactant is concentrate amount 0.05~0.5%, and reaction temperature is 105~170 DEG C, stirring speed
Degree is 100~800 revs/min, and oxygen presses 0.2~1.5MPa, and the reaction time is 0.5~3h, reaction end pH value 5.0 or more, in
Property leach key reaction have：
2PbS+4RSO3H+O2=2Pb (RSO3)2+S0+2H2O
PbS+2RSO3H+2Fe3+=2Pb (RSO3)2+S0+2Fe2++H2O
4Fe2++O2+6H2O=4FeOOH+8H+
R is CH in reaction equation3、C2H5。
2) above-mentioned neutral leachate is made into the sulfonic acid solutions of certain lead concentration with useless electric effusion, and electro-deposition obtains metallic lead
Plate and useless electric effusion.Electro-deposition leads part is：Current density is 80~400A/m2, 30~65 DEG C of electric effusion temperature.Electrodeposition lead mistake
Cheng Zhong is the moon with Lead initiated plate electrode, titanium plate or stainless steel plate using graphite cake, ti-supported lead dioxide electric net or titanium-based platinum guaze as anode plate
Pole plate；The cathode plate periphery is 1~3 centimetre longer than the anode plate.Electrolytic deposition process key reaction has：
4Pb(RSO3)2+2H2O=4Pb+O2+4RSO3H
3) above-mentioned neutral leaching residue (adjusts the electric effusion that gives up using sulfonic acid solutions, makes its free sulfonic with sulfonic acid leaching agent
Concentration is within the scope of 0.3~2.5mol/L) mixing, neutrality, which leaches the iron to precipitate and reacts to dissolve with sulfonic acid, enters solution,
Pressure oxidation leaching is carried out in the autoclave of certain temperature and oxygen pressure, and the neutral sulphur for leaching unreacted vulcanized lead is made to be aoxidized
At elementary sulfur, acidic leaching residue is entered, and lead dissolving enters solution.After solid-liquor separation, obtains acid leaching solution and soaked with acid
It slags tap.The condition of acidic leaching is：Leaching agent is mainly the sulfonic acid of useless electric effusion and supplement, free sulfonic a concentration of 0.3~
2.5mol/L, extraction temperature are 110~170 DEG C, and mixing speed is 200~800 revs/min, and oxygen presses 0.2~1.5MPa, when leaching
Between 0.5~3.0h, leaching terminal acidity be 0.1-0.8mol/L；Acidic leaching process key reaction has：
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 250g (its chemical composition such as table 1) is taken, acid leaching solution 1200mL is added, chemical composition is：
Pb2+110g/L, iron ion total concentration are 0.21mol/L, and dissociate a concentration of 0.4mol/L of pyrovinic acid；And the wooden sulphurs of 0.5g are added
Sour calcium is polytetrafluoroethylene (PTFE) in 2000mL autoclave liners, and mixing speed 550r/min is passed through oxygen and maintains pressure 0.6MPa,
React 2.5h at 130 DEG C of temperature, until solution ph 5.3, after iron ion total concentration is less than 4mg/L, Separation of Neutral leachate with
Neutral leaching residue.
The useless electric effusions of 1200mL are added in neutral leaching residue, and useless electric effusion ingredient is：Pb2+37g/L, pyrovinic acid concentration of dissociating
For 1.1mol/L, in 2000mL autoclaves, liner is polytetrafluoroethylene (PTFE), and mixing speed 500r/min is passed through oxygen and maintains pressure
0.6MPa reacts 1.2h at 140 DEG C of temperature.Reaction is completed to be separated by filtration acid leaching solution and acidic leaching residue.
The electric effusion 1500mL 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 80g/L.Ti-supported lead dioxide electric net is anode, and lead flake is cathode, pole span 4cm, electrodeposition
Temperature is 35 DEG C, current density 200A/m2Under the conditions of electrodeposition 16h, current efficiency reaches 99.90%.
Acidic leaching residue dry weight 131.0g, lead-in-dreg 1.56%, analysis result show the leaching rate of lead up to 98.32%, and
Noble silver, gold fully enter in leached mud.
Comparative example 1
Concentrate of lead sulfide ore 250g (its chemical composition such as table 1) is taken, acid leaching solution 1200mL is added, chemical composition is：
Pb2+110g/L, iron ion total concentration are 0.21mol/L, and dissociate a concentration of 0.4mol/L of pyrovinic acid；And the wooden sulphurs of 0.5g are added
Sour calcium is polytetrafluoroethylene (PTFE) in 2000mL autoclave liners, and mixing speed 550r/min is passed through oxygen and maintains pressure 1.2MPa,
React 2.5h at 180 DEG C of temperature, until solution ph 5.3, after iron ion total concentration is less than 4mg/L, Separation of Neutral leachate with
Neutral leaching residue.
The useless electric effusions of 1200mL are added in neutral leaching residue, and useless electric effusion ingredient is：Pb2+37g/L, pyrovinic acid concentration of dissociating
For 1.1mol/L, in 2000mL autoclaves, liner is polytetrafluoroethylene (PTFE), and mixing speed 500r/min is passed through oxygen and maintains pressure
1.2Mpa reacts 1.2h at 180 DEG C of temperature.Reaction is completed to be separated by filtration acid leaching solution and acidic leaching residue.
Acidic leaching residue dry weight 221.0g, lead-in-dreg 28.56%, analysis result show the leaching rate only 48.17% of lead, and
Noble silver has 45.64% to enter in leachate, this is that have part sulphur to be oxidized to sulfate radical, makes lead ion at PbSO4Into
In slag.
Claims (5)
1. the method that lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions, it is characterised in that：Including following step
Suddenly：
1) it after mixing concentrate of lead sulfide ore, surfactant with leaching agent containing sulfonic acid, is transferred in autoclave, oxygen is passed through into system
Gas, carries out neutral leaching, and solid-liquor separation obtains neutral leachate and neutral leaching residue；Neutral leaching condition is：It is leached containing sulfonic acid
The liquid-solid ratio of agent and concentrate of lead sulfide ore be 3mL/g~15mL/g, surfactant qualities be concentrate of lead sulfide ore quality 0.05~
0.5%, reaction temperature is 105~170 DEG C, and mixing speed is 100~800 revs/min, and oxygen presses 0.2~1.5MPa, and the reaction time is
0.5~3h, 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) neutral leaching residue described in is mixed with acid lixiviant, is transferred in autoclave, and oxygen is passed through into system, is carried out acid
It leaches, after 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；The condition of the acidic leaching is：Neutrality leaching
Slag tap with the liquid-solid ratio of acid lixiviant be 3mL/g~15mL/g, extraction temperature be 110~170 DEG C, mixing speed be 200~
800 revs/min, oxygen press 0.2~1.5MPa, extraction time be 0.5~3.0h, leach terminal point control system acidity be 0.1~
0.8mol/L；
4) acid leaching solution enters neutral leach next time as leaching agent containing sulfonic acid and uses, the acidic leaching residue recycling
Elementary sulfur and noble metal.
2. the method that lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions according to claim 1,
It is characterized in that：The leaching agent containing sulfonic acid includes pyrovinic acid and/or ethylsulfonic acid.
3. the method that lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions according to claim 1,
It is characterized in that：Surfactant used includes at least one of ligninsulfonate, o-phenylenediamine, m-phenylene diamine (MPD).
4. the method that lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions according to claim 1,
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 lead in concentrate of lead sulfide ore is leached in two sections of adverse current pressure oxidations of sulfonic acid solutions according to claim 1 or 4,
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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| CN110396608B (en) * | 2019-08-02 | 2021-06-18 | 中南大学 | Oxygen pressure 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 |
| CN112064062B (en) * | 2020-11-10 | 2021-02-12 | 矿冶科技集团有限公司 | Method for preparing crude lead by waste lead plaster without pre-desulfurization combined electrolysis |
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| CN101113490B (en) * | 2007-09-12 | 2010-05-19 | 昆明理工大学 | Method for leaching indium from indium sulfide concentrate |
| US9322105B2 (en) * | 2012-11-13 | 2016-04-26 | The University Of British Columbia | Recovering lead from a lead material including lead sulfide |
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