CN106636660A - Copper anode furnace slag comprehensive utilization method - Google Patents
Copper anode furnace slag comprehensive utilization method Download PDFInfo
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- CN106636660A CN106636660A CN201610966870.3A CN201610966870A CN106636660A CN 106636660 A CN106636660 A CN 106636660A CN 201610966870 A CN201610966870 A CN 201610966870A CN 106636660 A CN106636660 A CN 106636660A
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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
- C22B7/04—Working-up slag
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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
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a copper anode furnace slag comprehensive utilization method which comprises the steps of rough breaking and sorting, magnetic separation, fine grinding classification, strong magnetic separation, chlorination, copper powder replacement, neutralization for copper precipitation, acid splitting, copper extraction reverse extraction-copper electrodeposition with copper, neutralization for zinc precipitation and the like. Compared with the prior art, because the copper anode furnace slag comprehensive utilization method adopts a separation-smelting combined technique, most of copper and iron in slag of a copper anode furnace return to a copper smelting system and are recycled, through subsequent wet-process metallurgy, copper, zinc and noble metal in slag are recovered and enriched respectively, zinc precipitation liquid, cleaning liquid, acid splitting residues, and the like return to a chlorination process, no waste liquid or dangerous waste is generated, and the copper anode furnace slag comprehensive utilization has good economic benefits and environment benefits.
Description
Technical field
The invention belongs to copper, zinc and enrichment rare precious metal are reclaimed in Cu-S ore recycling, more particularly to copper anode furnace slag
Method.
Background technology
Copper ashes is the lime-ash produced during smelting, fusing of copper and copper alloy etc., is the important secondary resource of copper and zinc.
Part by weight, accounts for the 10%～80% of the quantity of slag with agglomerate and the metal of graininess in slag, and another part is powder
The metal of state or its oxide.Mainly then iron is separated with magnetic separation from the big grain metal of alligator coarse crushing screening at present
Property material, then Jing it is appropriate it is in small, broken bits after, with the thin clipped wire of gravity treatment recovery section.These metals can be with reduction melting into blister copper or copper
Alloy.Remain in the metal or its oxide that are powder in sand-lime.10%～20%, such as cupric is higher than 8% to content,
Some smelteries reclaim the dispensing as Copper making, and zinc in melting more enter in people's flue dust or slag.Choosing is gone after bulky grain metal
Slag ash content composition analysis result：Copper 7.77%, zinc 18.05%, silica 22.38%, aluminum oxide 13.48%, calcium oxide
3.56%th, magnesia 2.78%, di-iron trioxide 4.56%, manganese dioxide 0.23%, potassium oxide 0.1%, sodium oxide molybdena 0.37%,
Nickel 0.051%, carbon monoxide 0.004%, cadmium 0.005%, lead 0.35%.Material phase analysis show, copper, and two kinds of elements of zinc are with gold
Category and oxide form are present.Meanwhile, detected with ICP, containing noble metals such as a small amount of gold and palladium in anode copper stove slag.Cause
This, anode furnace slag has very high recovery value.
Anode furnace slag is typically processed using cremate dilution, using anode furnace slag as furnace cupola, shaft furnace or square stove
Raw material is processed, in furnace cupola, shaft furnace or square stove dilution process is carried out, reclaim copper and rare precious metal in slag, zinc is with cigarette
Dirt form is entered in cigarette ash.With the raising of national environmental protection and access threshold, furnace cupola, shaft furnace and square stove progressively list superseded name in
Record, other methods of disposal of anode furnace slag become study hotspot.
Hydrometallurgy has very big advantage in terms of valuable metal separation, if solving the waste water row in hydrometallurgy process
Problem is put, the disposal on anode furnace slag will be obtained great popularization and application by hydrometallurgy.
The content of the invention
The purpose of the present invention mainly solves the problems, such as copper anode furnace slag synthetical recovery, proposes to adopt choosing-smelting process integration, will
Most copper, iron in copper anode furnace slag returns copper metallurgy industry, and residual copper, zinc and noble metal are divided by hydrometallurgy
From and enrichment, the tail washings that the technique is produced can return original system, not only can guarantee that the recovery of valuable metal, and treatment of process streams
Journey is short, equipment is simple, small investment, upper detective, do not cause secondary pollution.
A kind of method of copper anode furnace comprehensive utilization of slag of the present invention is as follows：
Anode furnace slag is slightly broken and sieved, thick to break using jaw crusher or kibbler roll, screening is divided into
Into three granularities, point ratio is particle and -0.5mm little particles in+2mm bulky grains ,+0.5mm～-2mm, and wherein bulky grain returns copper
Smelting system；Middle particle carries out magnetic separation, and magnetic field intensity is 2500～3500Gs, obtains magnetisable material and namagnetic substance, magnetic
Material returns to copper metallurgy industry；Little particle and magnetic separation obtain namagnetic substance and carry out fine grinding, and fine grinding is using airflow milling or stirs
Mill is mixed, partition size is 200 mesh；- 200 mesh materials that detailed catalogue classification is obtained carry out strong magnetic using 10000～16000Gs magnetic separators
Choosing, obtains magnetisable material and namagnetic substance, and magnetisable material returns copper metallurgy industry；The namagnetic substance of high intensity magnetic separation carries out chlorine
Change, chlorination adopt sodium chloride, sodium chlorate and hydrochloric acid system, in system sodium chloride concentration be 200～300g/L, sodium chlorate addition
For 20～30g/L, the solid mass ratio of liquid is 2：1～4：1, reaction temperature is 50～80 DEG C, and the reaction time is 2～4 hours, is reacted
All the time hydrochloric acid control solution pH=0.5～1 is used in journey, chlorated liquid and chloride slag is obtained, chloride slag is focused on；According to chlorated liquid
Volume adds copper powder to enter line replacement, adds copper powder amount to be 0.5～2g/L, is filtrated to get your slag and the displacement of the noble metal of palladium containing gold and silver
Liquid afterwards；Displaced liquid adds sodium acid carbonate to be neutralized, and neutralization pH is 5～6, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes
Add sulfuric acid to carry out acidolysis, it is 1.5～2.5 finally to control pH, be filtrated to get acidolysis slag and acid hydrolysis solution, acidolysis slag returns chlorination work
Sequence；Acid hydrolysis solution carries out extraction back extraction, and raffinate returns hydrolysis procedure, and back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；In
Add sodium acid carbonate, adjustment pH=8～9 to carry out heavy zinc in the heavy copper liquid obtained with heavy copper, obtain heavy cadmia and heavy zinc liquid, heavy zinc
Slag cleaning obtains crude zinc and cleaning fluid, and cleaning fluid and heavy zinc liquid return chloride process.
Compared with prior art, due to present invention employs choosing-smelting process integration, the copper, iron in copper anode furnace slag is big
Part returns copper metallurgy industry, is reused, subsequently through hydrometallurgy, copper therein, zinc and noble metal obtaining respectively
Reclaim and be enriched with, heavy zinc liquid, cleaning fluid, acidolysis slag etc. return chloride process, without waste liquid and the useless generation of danger, with good economy
Benefit and environmental benefit.
The present invention has the circulation of relatively common and cheap simple for process, raw materials used and equipment, liquid and waste residue
Using and it is pollution-free the features such as.
Description of the drawings
Fig. 1 represents copper anode furnace comprehensive utilization of slag process chart；
Specific embodiment
Embodiment 1
By copper content be 5.34%, Zn content be 15.88%, gold content be 16.26g/t, silver content be 283.19g/t,
Palladium content is slightly broken and is sieved for the anode furnace slag of 24.24g/t, thick to break using jaw crusher or kibbler roll,
Screening is divided into into three granularities, and point ratio is particle and -0.5mm little particles in+2mm bulky grains ,+0.5mm～-2mm, wherein big
Grain returns copper metallurgy industry；Middle particle carries out magnetic separation, and magnetic field intensity is 2500Gs, obtains magnetisable material and namagnetic substance, magnetic
Property material returns to copper metallurgy industry；Little particle and magnetic separation obtain namagnetic substance and carry out fine grinding, fine grinding using airflow milling or
Ball-stirring mill, partition size is 200 mesh；- 200 mesh materials that detailed catalogue classification is obtained carry out high intensity magnetic separation using 10000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material return copper metallurgy industry；The namagnetic substance of high intensity magnetic separation carries out chlorination, chlorination
Using sodium chloride, sodium chlorate and hydrochloric acid system, sodium chloride concentration is 200g/L in system, and sodium chlorate addition is 20g/L, and liquid is solid
Mass ratio is 2：1, reaction temperature is 50 DEG C, and the reaction time is 2 hours, all the time with industrial hydrochloric acid control solution pH in course of reaction
=0.5, chlorated liquid and chloride slag are obtained, chloride slag is focused on；Chlorination is using indication in sodium chloride, sodium chlorate and hydrochloric acid system
Hydrochloric acid be above-mentioned technical hydrochloric acid, it is therefore an objective to maintain pH following examples all identical.
Add copper powder to enter line replacement according to chlorated liquid volume, add copper powder amount to be 0.5g/L, be filtrated to get palladium containing gold and silver expensive
Your slag of metal and displaced liquid；Displaced liquid add sodium acid carbonate be neutralized, neutralization pH be 5, be filtrated to get heavy copper ashes and
Heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid to carry out acidolysis, and it is 1.5 finally to control pH, is filtrated to get acidolysis slag and acidolysis
Liquid, acidolysis slag returns chloride process；Acid hydrolysis solution carries out extraction back extraction, and raffinate returns hydrolysis procedure, and back extraction obtains copper sulphate and enters
Row electrodeposition, obtains electro deposited copper；Sodium acid carbonate, adjustment pH=8 is added to carry out heavy zinc, sunk in the heavy copper liquid that the heavy copper of neutralization is obtained
Cadmia and heavy zinc liquid, heavy cadmia cleaning obtains crude zinc and cleaning fluid, and cleaning fluid and heavy zinc liquid return chloride process.Your slag gold content
12624g/t, silver content 197010g/t, palladium content 16738g/t.
Embodiment 2
By copper content be 5.71%, Zn content be 19.61%, gold content be 12.70g/t, silver content be 261.55g/t,
Palladium content is slightly broken and is sieved for the anode furnace slag of 18.84g/t, thick to break using jaw crusher or kibbler roll,
Screening is divided into into three granularities, and point ratio is particle and -0.5mm little particles in+2mm bulky grains ,+0.5mm～-2mm, wherein big
Grain returns copper metallurgy industry；Middle particle carries out magnetic separation, and magnetic field intensity is 3500Gs, obtains magnetisable material and namagnetic substance, magnetic
Property material returns to copper metallurgy industry；Little particle and magnetic separation obtain namagnetic substance and carry out fine grinding, fine grinding using airflow milling or
Ball-stirring mill, partition size is 200 mesh；- 200 mesh materials that detailed catalogue classification is obtained carry out high intensity magnetic separation using 16000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material return copper metallurgy industry；The namagnetic substance of high intensity magnetic separation carries out chlorination, chlorination
Using sodium chloride, sodium chlorate and hydrochloric acid system, sodium chloride concentration is 300g/L in system, and sodium chlorate addition is 30g/L, and liquid is solid
Mass ratio is 4：1, reaction temperature is 80 DEG C, and the reaction time is 4 hours, all the time with industrial hydrochloric acid control solution pH in course of reaction
=1, chlorated liquid and chloride slag are obtained, chloride slag is focused on；Add copper powder to enter line replacement according to chlorated liquid volume, add copper powder
Measure as 2g/L, your slag and displaced liquid of the noble metal of palladium containing gold and silver be filtrated to get；Displaced liquid adds sodium acid carbonate to be neutralized,
Neutralization pH is 6, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid to carry out acidolysis, finally controls pH
For 2.5, acidolysis slag and acid hydrolysis solution are filtrated to get, acidolysis slag returns chloride process；Acid hydrolysis solution carries out extraction back extraction, and raffinate is returned
Hydrolysis procedure, back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；Bicarbonate is added in the heavy copper liquid that the heavy copper of neutralization is obtained
Sodium, adjustment pH=9 carries out heavy zinc, obtains heavy cadmia and heavy zinc liquid, and heavy cadmia cleaning obtains crude zinc and cleaning fluid, cleaning fluid and heavy
Zinc liquid returns chloride process.Your slag gold content 12184g/t, silver content 135431g/t, palladium content 17880g/t.
Embodiment 3
By copper content be 6.56%, Zn content be 15.26%, gold content be 23.50g/t, silver content be 168.38g/t,
Palladium content is slightly broken and is sieved for the anode furnace slag of 11.20g/t, thick to break using jaw crusher or kibbler roll,
Screening is divided into into three granularities, and point ratio is particle and -0.5mm little particles in+2mm bulky grains ,+0.5mm～-2mm, wherein big
Grain returns copper metallurgy industry；Middle particle carries out magnetic separation, and magnetic field intensity is 3000Gs, obtains magnetisable material and namagnetic substance, magnetic
Property material returns to copper metallurgy industry；Little particle and magnetic separation obtain namagnetic substance and carry out fine grinding, fine grinding using airflow milling or
Ball-stirring mill, partition size is 200 mesh；- 200 mesh materials that detailed catalogue classification is obtained carry out high intensity magnetic separation using 12000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material return copper metallurgy industry；The namagnetic substance of high intensity magnetic separation carries out chlorination, chlorination
Using sodium chloride, sodium chlorate and hydrochloric acid system, sodium chloride concentration is 250g/L in system, and sodium chlorate addition is 25g/L, and liquid is solid
Mass ratio is 3：1, reaction temperature is 60 DEG C, and the reaction time is 2～4 hours, molten with technical hydrochloric acid control all the time in course of reaction
Liquid pH=0.8, obtains chlorated liquid and chloride slag, and chloride slag is focused on；Copper powder is added to enter line replacement according to chlorated liquid volume, plus
It is 1g/L to enter copper powder amount, is filtrated to get your slag and displaced liquid of the noble metal of palladium containing gold and silver；Displaced liquid adds sodium acid carbonate to enter
Row neutralization, neutralization pH is 5.5, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid to carry out acidolysis, most
It is 2 to control pH eventually, is filtrated to get acidolysis slag and acid hydrolysis solution, and acidolysis slag returns chloride process；Acid hydrolysis solution carries out extraction back extraction, raffinate
Liquid returns hydrolysis procedure, and back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；Carbon is added in the heavy copper liquid that the heavy copper of neutralization is obtained
Sour hydrogen sodium, adjustment pH=8.5 carries out heavy zinc, obtains heavy cadmia and heavy zinc liquid, and heavy cadmia cleaning obtains crude zinc and cleaning fluid, cleans
Liquid and heavy zinc liquid return chloride process.Your slag gold content 17357g/t, silver content 140087g/t, palladium content 12006g/t.
Embodiment 4
By copper content be 5.06%, Zn content be 18.99%, gold content be 16.92g/t, silver content be 180.18g/t,
Palladium content is slightly broken and is sieved for the anode furnace slag of 22.84g/t, thick to break using jaw crusher or kibbler roll,
Screening is divided into into three granularities, and point ratio is particle and -0.5mm little particles in+2mm bulky grains ,+0.5mm～-2mm, wherein big
Grain returns copper metallurgy industry；Middle particle carries out magnetic separation, and magnetic field intensity is 3500Gs, obtains magnetisable material and namagnetic substance, magnetic
Property material returns to copper metallurgy industry；Little particle and magnetic separation obtain namagnetic substance and carry out fine grinding, fine grinding using airflow milling or
Ball-stirring mill, partition size is 200 mesh；- 200 mesh materials that detailed catalogue classification is obtained carry out high intensity magnetic separation using 14000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material return copper metallurgy industry；The namagnetic substance of high intensity magnetic separation carries out chlorination, chlorination
Using sodium chloride, sodium chlorate and hydrochloric acid system, sodium chloride concentration is 280g/L in system, and sodium chlorate addition is 23g/L, and liquid is solid
Mass ratio is 3.5：1, reaction temperature is 70 DEG C, and the reaction time is 2.5 hours, molten with technical hydrochloric acid control all the time in course of reaction
Liquid pH=0.7, obtains chlorated liquid and chloride slag, and chloride slag is focused on；Copper powder is added to enter line replacement according to chlorated liquid volume, plus
It is 1.5g/L to enter copper powder amount, is filtrated to get your slag and displaced liquid of the noble metal of palladium containing gold and silver；Displaced liquid adds sodium acid carbonate
It is neutralized, neutralization pH is 5.5, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid to carry out acidolysis,
The final pH that controls is 2, is filtrated to get acidolysis slag and acid hydrolysis solution, and acidolysis slag returns chloride process；Acid hydrolysis solution carries out extraction back extraction, extraction
Extraction raffinate returns hydrolysis procedure, and back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；Add in the heavy copper liquid that the heavy copper of neutralization is obtained
Sodium acid carbonate, adjustment pH=8.8 carries out heavy zinc, obtains heavy cadmia and heavy zinc liquid, and heavy cadmia cleaning obtains crude zinc and cleaning fluid, clearly
Washing lotion and heavy zinc liquid return chloride process.Your slag gold content 15043g/t, silver content 148366g/t, palladium content 17403g/t.
Claims (2)
1. a kind of method of anode furnace comprehensive utilization of slag, it is characterised in that step is as follows：
(1) thick broken screening：Anode furnace slag is slightly broken and sieved, it is thick to break using jaw crusher or kibbler roll,
Screening is divided into into three granularities, and point ratio is particle and -0.5mm little particles in+2mm bulky grains ,+0.5mm～-2mm, wherein big
Grain returns copper metallurgy industry；
(2) magnetic separation：Step (1) obtains middle particle and carries out magnetic separation, and magnetic field intensity is 2500～3500Gs, obtains magnetisable material and non-
Magnetisable material, magnetisable material returns to copper metallurgy industry；
(3) fine grinding classification：The little particle and step (2) that step (1) is obtained obtains namagnetic substance carries out fine grinding, and fine grinding adopts gas
Stream mill or Ball-stirring mill, partition size is 200 mesh；
(4) high intensity magnetic separation：- 200 mesh materials are obtained in step (3) carries out high intensity magnetic separation, and magnetic field intensity is 10000～16000Gs, is obtained
To magnetisable material and namagnetic substance, magnetisable material return copper metallurgy industry；
(5) chlorination：The namagnetic substance obtained in step (3) carries out chlorination, obtains chlorated liquid and chloride slag, and chloride slag is concentrated
Process；
(6) copper powder displacement：Add copper powder to enter line replacement in the chlorated liquid obtained to step (5), add copper powder amount to be 0.5～2g/
L, is filtrated to get your slag and displaced liquid of the noble metal of palladium containing gold and silver；
(7) heavy copper is neutralized：The displaced liquid obtained to step (6) adds sodium acid carbonate to be neutralized, and neutralization pH is 5～6, is filtered
Obtain heavy copper ashes and heavy copper liquid；
(8) acidolysis：The heavy copper ashes obtained to step (7) adds sulfuric acid to carry out acidolysis, and it is 1.5～2.5 finally to control pH, is filtered
To acidolysis slag and acid hydrolysis solution, acidolysis slag return chloride process；
(9) copper extraction back extraction+copper electrodeposition：The acid hydrolysis solution obtained to step (8) carries out extraction back extraction, and raffinate returns acidolysis work
Sequence, back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；
(10) heavy zinc is neutralized：Sodium acid carbonate, adjustment pH=8～9 is added to carry out heavy zinc, obtain in the heavy copper liquid obtained to step (7)
To heavy cadmia and heavy zinc liquid, heavy cadmia cleaning obtains crude zinc and cleaning fluid, and cleaning fluid and heavy zinc liquid return chloride process.
2. a kind of method of anode furnace comprehensive utilization of slag as claimed in claim 1, it is characterised in that chlorination in step (5) is adopted
With sodium chloride, sodium chlorate and hydrochloric acid system, sodium chloride concentration is 200～300g/L in system, sodium chlorate addition is 20～
30g/L, the solid mass ratio of liquid is 2：1～4：1, reaction temperature is 50～80 DEG C, and the reaction time is 2～4 hours, is begun in course of reaction
Hydrochloric acid control solution pH=0.5～1 is used eventually.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537676A (en) * | 2017-08-30 | 2018-01-05 | 四川深蓝环保科技有限公司 | A kind of method that iron is selected in flyash |
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| CN103882240A (en) * | 2014-04-16 | 2014-06-25 | 芒市海华开发有限公司 | Method and equipment for extracting gold and silver from smelting slag |
| WO2015143574A1 (en) * | 2014-03-28 | 2015-10-01 | ALTAMIRANO MUNOZ, Francisca | Method for recovering copper, molybdenum and other materials from foundry slag |
| CN105177301A (en) * | 2015-08-28 | 2015-12-23 | 商洛学院 | Technology for recycling and refining furnace clinker of lead and zinc metallurgical furnace |
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| JP2002018395A (en) * | 2000-07-06 | 2002-01-22 | Taiheiyo Cement Corp | Treating method for waste |
| CN102732735A (en) * | 2012-07-20 | 2012-10-17 | 阳谷祥光铜业有限公司 | Method for recovering valued metals from melting slag of copper anode slime Kaldo furnace |
| WO2015143574A1 (en) * | 2014-03-28 | 2015-10-01 | ALTAMIRANO MUNOZ, Francisca | Method for recovering copper, molybdenum and other materials from foundry slag |
| CN103882240A (en) * | 2014-04-16 | 2014-06-25 | 芒市海华开发有限公司 | Method and equipment for extracting gold and silver from smelting slag |
| CN105177301A (en) * | 2015-08-28 | 2015-12-23 | 商洛学院 | Technology for recycling and refining furnace clinker of lead and zinc metallurgical furnace |
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| CN107537676A (en) * | 2017-08-30 | 2018-01-05 | 四川深蓝环保科技有限公司 | A kind of method that iron is selected in flyash |
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