CN109837396A - A kind of wet process of kiln slag iron ore concentrate utilizes method - Google Patents
A kind of wet process of kiln slag iron ore concentrate utilizes method Download PDFInfo
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Abstract
The present invention relates to a kind of wet processes of kiln slag iron ore concentrate to utilize method；Belong to metallurgical technology field.For the present invention using zinc hydrometallurgy kiln slag iron ore concentrate as raw material, aqueous hydrochloric acid solution enters the valuable metals such as iron, silver, copper, lead, zinc, arsenic in kiln slag iron ore concentrate in leachate as leaching agent, two sections of counterflow leachings；Leachate is purified using metal iron powder displacement, the heavy techniques such as arsenic and sulfide precipitation of control pH value, the valuable metals such as separation copper, silver, lead, zinc, arsenic, liquid is pure FeCl after purification2Its spray-wall interaction is obtained Fe by aqueous solution2O3The HCl gas of powder, generation is absorbed with water, is regenerated as hydrochloric acid and is returned to leaching process.The present invention has the advantage of environmental protection, economic, energy saving, high resource utilization, is convenient for industrialization production.
Description
Technical field
The present invention relates to a kind of wet processes of kiln slag iron ore concentrate to utilize method；Belong to metallurgical technology field.
Background technique
China's metallic zinc yield in 2011 is up to 4,460,000 tons, wherein about 85% uses wet production.Zinc hydrometallurgy has conventional leaching
Out, the kinds of processes such as high temperature high acidic oils, normal pressure and hyperbaric oxygen leaching, are applied in China, wherein conventional extract technology produces
Amount accounts for about the 50% of China's wet process zinc yield.In conventional extract technology, roasted ore through neutral and low sour two sections of counterflow leachings,
Middle Pb, Au, Ag, In, Ge, Ga and 60%Cu, 30%Cd and 15% Zn enter in leached mud.Leached mud uses waelz process
Processing, that is, the coke powder of supplying 45~55%, is sent into rotary kiln after mixing after drying, under 1100~1300 DEG C of high temperature, Zn, Pb,
The reduction volatilizations output secondary zinc oxide such as Cd, the clinker of semi-molten state is from kiln tail discharge water quenching at kiln slag.
Main valuable element ingredient (mass fraction) in above-mentioned kiln slag are as follows: Cu 0.7%~1.2%, Fe 35%~40%,
C 15%~18%, 0.1~0.3g/t of Au, 250~300g/t of Ag, 100~250g/t of In, 100~300g/t of Ge.Using
Conventional extract technology, every production 1t electricity zinc about output leached mud 1.05t, kiln slag 0.8t.China about 1,500,000 t of output kiln slag every year.
Kiln slag hardness height, fine size, ingredient, object phase and its embedding cloth state complex are studied after many decades, and comprehensive recycling process is still
It does not make a breakthrough, previous general stockpiling processing results in waste of resources and pollutes environment.
In recent years, Some Domestic enterprise handles above-mentioned kiln slag using the physical separation method that weight, magnetic separation etc. combine, respectively
The substances such as output coke powder, iron ore concentrate and tailing.Coke powder is used for manufacture of cement as fuel utilization, tailing.It is enriched in iron ore concentrate
The valuable metals such as Cu, Ag, In, iron content is up to mass percentage 65% or so.Currently, there are two types of purposes for this kind of iron ore concentrate: the
One is being used as flux to use in sintering-Lead Smelting in Blast Furnace technique, this obtains the valuable metals such as Cu, Ag and In therein
To partially recycled, but as sintering-Lead Smelting in Blast Furnace technique is phased out due to the reasons such as energy consumption is high, pollution is big, this aspect
Application tend to disappear；Iron-smelting raw material is used as second, but since the harmful elements content such as its S, As is higher, so can only lack
Amount is mixed, and the valuable metals such as this kind of iron ore concentrate price generally lower while contained therein copper, silver, indium are in ironmaking processes
It cannot be recycled, be resulted in waste of resources.
For the synthetical recovery of zinc hydrometallurgy kiln slag iron ore concentrate, also once two kinds of new techniques of experimental study: the first is
Using sulfuric acid leaching, after leachate recovering copper and dissipated metal element, polyaluminum sulfate iron product is manufactured.Due to sulfuric acid leaching
In only part iron, copper, zinc enter leachate, most silver, lead and part copper, zinc are remained in leached mud, cannot be recycled
Rare precious metal and other valuable elements.And polyaluminum sulfate iron product market is smaller, this technique is not able to achieve industrialized production；The
Two kinds are by the founding of kiln slag iron ore concentrate into iron anode, are handled using electrolysis process it, cathode output pure iron product conduct
Powder metallurgy raw material utilizes, other valuable elements are recycled from electrolyte or the earth of positive pole respectively.This technological difficulty is big, adds
Pure iron product marketing limitation, economic benefit is difficult to ensure, is not also applied industrially.
In conclusion zinc hydrometallurgy kiln slag iron ore concentrate yield is big, valuable element content is high, it is a kind of higher metal of value
Resource, but so far still without a kind of preferable technique, the Comprehensive recycling to realize resource is handled it.Just
It is in this context, to have invented a kind of method of comprehensive utilization of zinc hydrometallurgy kiln slag iron ore concentrate.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of wet processes of kiln slag iron ore concentrate to utilize method.
A kind of wet process of kiln slag iron ore concentrate of the present invention utilizes method, includes the following steps:
Step 1 zinc hydrometallurgy kiln slag iron ore concentrate salt Ore Leaching
Weak-acid leaching processing, gained Weak-acid leaching are carried out to zinc hydrometallurgy kiln slag iron ore concentrate with the hydrochloric acid of 0.5~1mol/L
Liquid is spare, and gained Weak-acid leaching slag carries out high acidic oils with the hydrochloric acid of 4~6mol/L, and the return of leachate obtained by high acidic oils is used for
Weak-acid leaching, high acidic oils gained leached mud is in the processing of sulfuric acid process；
Step 2 iron replacement copper, silver
The pH value of above-mentioned Weak-acid leaching liquid is transferred to 0.5~1.5, is charged with iron powder, liquid is solid after carrying out displacement reaction
Separation, obtains silver-bearing copper slag and displaced liquid；The additional amount of iron powder is to displace all silver ions and copper in the Weak-acid leaching liquid
1.1~2.5 times of the theoretical amount of fe needed for ion；
Step 3 sinks arsenic
The pH value of displaced liquid is transferred to 2.0~3.5, heavy arsenic processing is carried out at 60~95 DEG C, heavy arsenic slag is obtained and sinks
Liquid after arsenic；
Step 4 lead, zinc sulfide precipitation
Vulcanizing agent is added after heavy arsenic in liquid, the lead in solution, zinc ion is made to generate sulfide precipitation, obtain lead cadmia and
Liquid after purification；The additional amount of vulcanizing agent be by after the heavy arsenic in liquid all lead ions and zinc ion sulfide precipitation at lead cadmia institute
Need 2~6 times of theoretical amount；The vulcanizing agent is the metal sulfide or H of divalent sulfur2S；
Step 5 FeCl2Aqueous solution spray-wall interaction
Automiser spray will be packed by liquid after purification, using oxygen-containing gas as carrier gas, in 400~1000 DEG C of progress spray pyrolysis,
Obtain Fe2O3Concentrated hydrochloric acid is made in powder and HCl gas, HCl gas after water absorbs, and returns to high acidic oils process and uses.
Main component is as follows by percentage to the quality for the zinc hydrometallurgy kiln slag iron ore concentrate:
Iron 40~68%,
Copper 0.5~5%,
Zinc 0.5~5%,
Lead 0.5~5%,
Arsenic 0.1~5%,
Sulphur 3.0%~10%,
Al2O31%~3%,
SiO22.3~6.8%；
It further include silver in the iron ore concentrate, silver-colored content is 10~1000g/t.
Leaching described in step 1 is counterflow leaching, and when Weak-acid leaching, control extraction temperature is room temperature to 90 DEG C, the time to be
30~240min, liquid-solid ratio are 5:1~20:1ml/g；When high acidic oils, control extraction temperature is room temperature to 80 DEG C, extraction time
It is 5:1~20:1ml/g for 30~180min, liquid-solid ratio；After two sections of counterflow leachings, 99.0% or more silver, 95.0% with
On copper, 55.0% or more zinc, 99.0% or more lead, 90.0% or more arsenic, 90.0% or more iron enter leachate
In.
In step 2, the specific surface area of iron powder used is 0.17~0.36m2/g；When displacement reaction, controlled at room temperature
It is 20~120min to 50 DEG C, time.
In step 3, pass through control solution ph and 30~240min of temperature.
In step 4, when lead, zinc sulfide precipitation, the temperature for controlling solution is room temperature to 80 DEG C.
In step 4, vulcanizing agent is the metal sulfide or hydrogen sulfide of divalent sulfur, and the metal sulfide of the divalent sulfur is
Ferrous sulfide or pyrite, FeS in the pyrite2Mass percentage >=90%.
In step 4, the time of sulfide precipitation lead cadmia is 60~240min；The quality percentage of Zn contains in the lead cadmia
Measure mass percentage > 20% of mass percentage > 30%, S of > 45%, Pb.
It is 400~1000 DEG C in temperature, under the conditions of oxidizing atmosphere, by FeCl in step 52Solution spray-wall interaction is
Fe2O3And HCl, HCl gas prepare hydrochloric acid and return to leaching.
Specific embodiment
Technical solution of the present invention is described in detail below, wherein the percentage composition is mass number.
Main iron content mass percentage 40%~68%, 10~1000g/t of silver content, copper in raw material of the present invention
Mass percentage 0.5%~5%, zinc mass percentage 0.5%~5%, lead mass percentage 0.5%~5%, arsenic matter
Measure percentage composition 0.1%~5%, sulphur mass percentage 2.3%~10%, Al2O3Mass percentage 1%~3%, SiO2
Mass percentage 2.3%~6.8%.
It is the embodiment of the present invention below.
Embodiment 1:
Using zinc hydrometallurgy kiln slag iron ore concentrate as raw material, the main component of raw material are as follows: Fe 40%, Ag 10g/t, Cu
5.0%, Zn 5.0%, Pb 5.0%, As 5.0%, Al2O31.0%, S 10.0%, SiO26.8%；
Kiln slag iron ore concentrate is leached at room temperature, and the concentration of hydrochloric acid is 0.5mol/L, liquid-solid ratio 10:1ml/ when Weak-acid leaching
G, extraction time 240min；Gained Weak-acid leaching liquid is spare, and gained Weak-acid leaching slag is by liquid-solid ratio with the hydrochloric acid of 3mol/L
20:1ml/g carries out high acidic oils 180min, and leachate concentration of hydrochloric acid is 0.65mol/L after high acidic oils, can return to Weak-acid leaching
Process continues to leach according to Weak-acid leaching condition, and leached mud obtained by high acidic oils is used for roasting technique；Through Weak-acid leaching and peracid
After leaching, the leaching rate that the leaching rate of Fe is 92.21%, Ag in raw material is 98.95%, and the leaching rate of copper is 95.07%, Pb's
The leaching rate that the leaching rate that leaching rate is 99.34%, As is 88.57%, Zn is 57.92%；
The pH value of Weak-acid leaching liquid is 1.5 at this time, requirement when meeting reduction silver, copper to solution ph, then in room temperature
Under, into above-mentioned Weak-acid leaching liquid be added metal iron powder carry out displacement reaction 120min, be then separated by solid-liquid separation, obtain silver-bearing copper slag and
Displaced liquid, the additional amount of iron powder are to displace the reason of fe needed for all silver ions and copper ion in the Weak-acid leaching liquid
By 1.5 times of dosage, after iron powder reducing, silver-colored reduction rate is 99.1% in solution, and the reduction rate of copper is 99.0%；
The pH value of displaced liquid is 2.0 at this time, and requirement when meeting heavy arsenic to solution ph then carries out displaced liquid
60 DEG C are warming up to, heavy arsenic processing 240min is carried out, liquid after arsenic slag and heavy arsenic is obtained by filtration；After heavy arsenic processing, the removal rate of arsenic
It is 95.42%, the arsenic slag is ferric arsenate or scorodite；
FeS is charged with after liquid after heavy arsenic is warming up to 80 DEG C2Mass percentage >=90% pyrite carry out
Vulcanize heavy lead zinc and handle 240min, obtains liquid after lead cadmia and purification；The additional amount of pyrite is will be after the heavy arsenic in liquid
All lead ions and zinc ion sulfide precipitation are at 5 times of theoretical amount needed for lead cadmia；Sulfide precipitation at lead cadmia simultaneously
Energy removes remaining arsenic, and after vulcanizing heavy lead zinc processing, after heavy arsenic in liquid, the removal rate that the removal rate of lead is 99.95%, Zn is
97.55%, after heavy arsenic processing and vulcanizing heavy lead zinc processing, the total removal rate of arsenic reaches 99.8%；
Liquid will be fitted into automiser spray and be atomized as fine mist after purification, in air atmosphere, reaction temperature is 800 DEG C,
Thermally decompose to yield Fe2O3Powder and HCl gas, recycling HCl gas are made hydrochloric acid solution and return to leaching process.
Embodiment 2:
Using zinc hydrometallurgy kiln slag iron ore concentrate as raw material, the main component of raw material are as follows: Fe 55.0%, Ag 1000g/t, Cu
0.5%, Zn 5.0%, Pb 5.0%, As 3.5%, Al2O32.0%, S 5.0%, SiO24.6%, remaining is each element oxygen
Oxygen in compound；Kiln slag iron ore concentrate is leached at 60 DEG C, the concentration of hydrochloric acid is 2.5mol/L when Weak-acid leaching, liquid-solid ratio 10:
1ml/g, extraction time 180min；Gained Weak-acid leaching liquid is spare, and gained Weak-acid leaching slag is solid by liquid with the hydrochloric acid of 5mol/L
Than carrying out high acidic oils 30min for 5:1ml/g, leachate concentration of hydrochloric acid is 2.6mol/L after high acidic oils, can return to low acidleach
Process out continues to leach according to Weak-acid leaching condition, and leached mud obtained by high acidic oils is used for roasting technique；Through Weak-acid leaching and height
After Ore Leaching, the leaching rate that the leaching rate of Fe is 91.36%, Ag in raw material is 99.95%, and the leaching rate of copper is 96.34%, Pb
Leaching rate be 99.55%, As leaching rate be 90.54%, Zn leaching rate be 60.79%；
The pH value of Weak-acid leaching liquid is 1.5 at this time, requirement when meeting reduction silver, copper to solution ph, then at 40 DEG C
Under, into above-mentioned Weak-acid leaching liquid be added metal iron powder carry out displacement reaction 60min, be then separated by solid-liquid separation, obtain silver-bearing copper slag and
Displaced liquid, the additional amount of iron powder are to displace the reason of fe needed for all silver ions and copper ion in the Weak-acid leaching liquid
By 1.1 times of dosage, after iron powder reducing, silver-colored reduction rate is 99.95% in solution, and the reduction rate of copper is 99.95%；
The pH value of displaced liquid is 2.4 at this time, adjusts the pH value of displaced liquid to after 3.0, is warming up to 95 DEG C, carries out heavy arsenic
30min is handled, liquid after arsenic slag and heavy arsenic is obtained by filtration；After heavy arsenic processing, the removal rate of arsenic is 99.0%, and the arsenic slag is arsenic
Sour iron or scorodite；
Liquid after heavy arsenic is passed through H2S gas carries out vulcanizing heavy lead zinc processing 240min, obtains liquid after lead cadmia and purification；H2S
Additional amount be by after the heavy arsenic in liquid all lead ions and zinc ion sulfide precipitation at 6 of theoretical amount needed for lead cadmia
Times；Remaining arsenic can be also removed simultaneously at lead cadmia in sulfide precipitation, and after vulcanizing heavy lead zinc processing, after heavy arsenic in liquid, lead is gone
Except the removal rate that rate is 99.95%, Zn is 97.55%, after heavy arsenic processing and vulcanizing heavy lead zinc processing, the total removal rate of arsenic reaches
To 99.99%；
Liquid after purification is fitted into automiser spray and is atomized as fine mist, in pure oxygen atmosphere, reaction temperature 400
DEG C, thermally decompose to yield Fe2O3Powder and HCl gas, recycling HCl gas are made hydrochloric acid solution and return to leaching process.
Claims (4)
1. a kind of wet process of kiln slag iron ore concentrate utilizes method, it is characterised in that include the following steps:
Step 1 zinc hydrometallurgy kiln slag iron ore concentrate salt Ore Leaching
Weak-acid leaching processing is carried out to zinc hydrometallurgy kiln slag iron ore concentrate with the hydrochloric acid of 0.5~1mol/L, gained Weak-acid leaching liquid is standby
With gained Weak-acid leaching slag carries out high acidic oils with the hydrochloric acid of 4~6mol/L, and leachate obtained by high acidic oils, which returns, is used for low acid
It leaches, leached mud obtained by high acidic oils is in the processing of sulfuric acid process；
The zinc hydrometallurgy kiln slag iron ore concentrate includes following main component by percentage to the quality:
Iron: 40%~68%,
Copper 0.5%~5%,
Zinc 0.5%~5%,
Lead 0.5%~5%,
Arsenic 0.1%~5%,
Sulphur 3.0%~10%,
Al2O31%~3%,
SiO22.3%~6.8%；
It further include silver in the iron ore concentrate, silver-colored content is 10~1000g/t；
Step 2 iron replacement copper, silver
The pH value of above-mentioned Weak-acid leaching liquid is transferred to 0.5~1.5, iron powder is charged with, carries out solid-liquor separation after displacement reaction,
Obtain silver-bearing copper slag and displaced liquid；The additional amount of iron powder is displaces all silver ions and copper ion institute in the Weak-acid leaching liquid
Need 1.1~2.5 times of the theoretical amount of fe；
Step 3 sinks arsenic
The pH value of displaced liquid is transferred to 2.0~3.5, heavy arsenic processing is carried out at 60~95 DEG C, after obtaining heavy arsenic slag and heavy arsenic
Liquid；
Step 4 lead, zinc sulfide precipitation
Vulcanizing agent is added after sinking arsenic in liquid, makes lead, zinc ion in solution generate sulfide precipitation, obtains lead cadmia and purification
Liquid afterwards；The additional amount of vulcanizing agent be by after the heavy arsenic in liquid all lead ions and zinc ion sulfide precipitation at reason needed for lead cadmia
By 2~6 times of dosage；The vulcanizing agent is the metal sulfide or H of divalent sulfur2S；
Step 5 FeCl2Aqueous solution spray-wall interaction
Liquid is packed into automiser spray and, in 400~1000 DEG C of progress spray pyrolysis, is obtained using oxygen-containing gas as carrier gas after purifying
Fe2O3Concentrated hydrochloric acid is made in powder and HCl gas, HCl gas after water absorbs, and returns to high acidic oils process and uses.
2. a kind of wet process of kiln slag iron ore concentrate according to claim 1 utilizes method, it is characterised in that:
Leaching described in step 1 is counterflow leaching, when Weak-acid leaching, control extraction temperature be 30 room temperature to 90 DEG C, the time~
240min, liquid-solid ratio are 5:1~20:1ml/g；When high acidic oils, control extraction temperature is room temperature to 80 DEG C, extraction time 30
~180min, liquid-solid ratio are 5:1~20:1ml/g；
In step 2, the specific surface area of iron powder used is 0.17~0.36m2/g；When displacement reaction, controlled at room temperature to 50
DEG C, the time be 20~120min；
In step 3, the heavy arsenic slag is ferric arsenate or scorodite.
3. a kind of wet process of kiln slag iron ore concentrate according to claim 1 utilizes method, it is characterised in that: in step 4, lead,
When zinc sulfide precipitation, the temperature for controlling solution is room temperature to 80 DEG C.
4. a kind of wet process of kiln slag iron ore concentrate according to claim 1 utilizes method, it is characterised in that: in step 4, institute
The metal sulfide for stating divalent sulfur is ferrous sulfide or pyrite, FeS in the pyrite2Mass percentage >=90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110550786A (en) * | 2019-10-18 | 2019-12-10 | 广西森合高新科技股份有限公司 | Waste liquid treatment process |
| CN111349790A (en) * | 2020-03-30 | 2020-06-30 | 北京矿冶科技集团有限公司 | Method for reducing arsenic content in copper smelting soot leaching slag |
-
2017
- 2017-11-29 CN CN201711222033.0A patent/CN109837396A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110550786A (en) * | 2019-10-18 | 2019-12-10 | 广西森合高新科技股份有限公司 | Waste liquid treatment process |
| CN111349790A (en) * | 2020-03-30 | 2020-06-30 | 北京矿冶科技集团有限公司 | Method for reducing arsenic content in copper smelting soot leaching slag |
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