CN106636660B - A kind of method of copper anode furnace comprehensive utilization of slag - Google Patents
A kind of method of copper anode furnace comprehensive utilization of slag Download PDFInfo
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- CN106636660B CN106636660B CN201610966870.3A CN201610966870A CN106636660B CN 106636660 B CN106636660 B CN 106636660B CN 201610966870 A CN201610966870 A CN 201610966870A CN 106636660 B CN106636660 B CN 106636660B
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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
A kind of method of copper anode furnace comprehensive utilization of slag, it is related to thick broken screening, magnetic separation, fine grinding classification, high intensity magnetic separation, chlorination, copper powder displacement, neutralizes heavy copper, acidolysis, copper extraction back extraction copper electro deposited copper, neutralize the techniques such as heavy zinc.Compared with prior art, because present invention employs selecting smelting combination technique, copper, iron in copper anode furnace clinker largely return to copper metallurgy industry, it is reused, follow-up pass through hydrometallurgy, the return chloride process such as zinc liquid, cleaning fluid, acidolysis slag is sunk in copper, zinc and noble metal therein being recycled and being enriched with respectively, produced without waste liquid and dangerous waste, there is good economic benefit and environmental benefit.
Description
Technical field
The invention belongs to Cu-S ore recycling, more particularly to copper anode furnace clinker recovery copper, zinc and enrichment rare precious metal
Method.
Background technology
Copper ashes is caused lime-ash during the smelting of copper and copper alloy, fusing etc., is the important secondary resource of copper and zinc.
Part by weight, accounts for the 10%~80% of the quantity of slag, another part is powder with agglomerate and the metal of graininess in slag
The metal of state or its oxide.Big grain metal mainly is screened from alligator coarse crushing at present, iron is then separated with magnetic separation
Property material, then through 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.It is powdered metal or its oxide to remain in sand-lime.Content is higher than 8% in 10%~20%, such as cupric,
Some smelteries reclaim dispensing as Copper making, and zinc in melting more enter in people's flue dust or slag.After bulky grain metal is removed in choosing
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 shows that copper, two kinds of elements of zinc are with gold
Category and oxide form are present.Meanwhile detected with ICP, the noble metal such as a small amount of gold and palladium is contained in anode copper stove clinker.Cause
This, anode furnace clinker has very high recovery value.
Anode furnace clinker is typically handled using cremate dilution, using anode furnace clinker as furnace cupola, shaft furnace or square stove
Raw material is handled, dilution processing is carried out in furnace cupola, shaft furnace or square stove, reclaims copper and rare precious metal in clinker, zinc is with cigarette
Dirt form enters in cigarette ash.With the raising of national environmental protection and access threshold, furnace cupola, shaft furnace and square stove are progressively included in superseded name
Record, other methods of disposal of anode furnace clinker turn into 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 clinker 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 clinker synthetical recovery, and proposition uses choosing-smelting process integration, will
Most copper, iron in copper anode furnace clinker return to copper metallurgy industry, and residual copper, zinc and noble metal are divided by hydrometallurgy
From and enrichment, tail washings can return to original system caused by the technique, 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, does 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 clinker slightly break and sieve, thick break uses jaw crusher or kibbler roll, and screening is divided into
Into three granularities, a point ratio is+2mm bulky grains, particle and -0.5mm little particles in+0.5mm~-2mm, and wherein bulky grain returns to 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 is classified to obtain carry out strong magnetic using 10000~16000Gs magnetic separators
Choosing, obtains magnetisable material and namagnetic substance, and magnetisable material returns to copper metallurgy industry；The namagnetic substance of high intensity magnetic separation carries out chlorine
Change, chlorination uses sodium chloride, sodium chlorate and hydrochloric acid system, and sodium chloride concentration is 200~300g/L in system, 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, obtains chlorated liquid and chloride slag, chloride slag focuses on；According to chlorated liquid
Volume adds copper powder and enters line replacement, and it is 0.5~2g/L to add copper powder amount, 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 and neutralized, and it is 5~6 to neutralize pH, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes
Add sulfuric acid and carry out acidolysis, it is 1.5~2.5 finally to control pH, is filtrated to get acidolysis slag and acid hydrolysis solution, and acidolysis slag returns to chlorination work
Sequence；Acid hydrolysis solution carries out extraction back extraction, and raffinate returns to hydrolysis procedure, and back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；In
Sodium acid carbonate is added in the heavy copper liquid obtained with heavy copper, adjustment pH=8~9 carry out heavy zinc, obtain heavy cadmia and heavy zinc liquid, heavy zinc
Slag cleans to obtain crude zinc and cleaning fluid, and cleaning fluid and heavy zinc liquid return to chloride process.
Compared with prior art, because present invention employs choosing-smelting process integration, the copper, iron in copper anode furnace clinker are big
Part returns to copper metallurgy industry, is reused, subsequently by hydrometallurgy, copper, zinc and noble metal therein obtaining respectively
Recovery and enrichment, heavy zinc liquid, cleaning fluid, acidolysis slag etc. return to chloride process, and no waste liquid and dangerous waste produce, and have good economy
Benefit and environmental benefit.
The present invention has relatively common and cheap simple for process, raw materials used and equipment, liquid and waste residue circulation
Using and it is pollution-free the features such as.
Brief description of the drawings
Fig. 1 represents copper anode furnace comprehensive utilization of slag process chart；
Embodiment
Embodiment 1
Be 5.34% by copper content, Zn content 15.88%, gold content 16.26g/t, silver content 283.19g/t,
The anode furnace clinker that palladium content is 24.24g/t slightly break and sieve, slightly broken to use jaw crusher or kibbler roll,
Screening is divided into three granularities, and a point ratio is+2mm bulky grains, particle and -0.5mm little particles in+0.5mm~-2mm, wherein big
Grain returns to copper metallurgy industry；Middle particle carries out magnetic separation, magnetic field intensity 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 are 200 mesh；- 200 mesh materials that detailed catalogue is classified to obtain carry out high intensity magnetic separation using 10000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material returns to 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 focuses on；Chlorination uses signified 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.
Copper powder is added according to chlorated liquid volume and enters line replacement, and it is 0.5g/L to add copper powder amount, and it is expensive to be filtrated to get palladium containing gold and silver
Your slag and displaced liquid of metal；Displaced liquid add sodium acid carbonate neutralized, neutralize pH be 5, be filtrated to get heavy copper ashes and
Heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid and carries out acidolysis, and it is 1.5 finally to control pH, is filtrated to get acidolysis slag and acidolysis
Liquid, acidolysis slag return to chloride process；Acid hydrolysis solution carries out extraction back extraction, and raffinate returns to hydrolysis procedure, and back extraction obtains copper sulphate and entered
Row electrodeposition, obtains electro deposited copper；Neutralize and sodium acid carbonate is added in the heavy copper liquid that heavy copper obtains, adjustment pH=8 carries out heavy zinc, sunk
Cadmia and heavy zinc liquid, heavy cadmia clean to obtain crude zinc and cleaning fluid, and cleaning fluid and heavy zinc liquid return to chloride process.Your slag gold content
12624g/t, silver content 197010g/t, palladium content 16738g/t.
Embodiment 2
Be 5.71% by copper content, Zn content 19.61%, gold content 12.70g/t, silver content 261.55g/t,
The anode furnace clinker that palladium content is 18.84g/t slightly break and sieve, slightly broken to use jaw crusher or kibbler roll,
Screening is divided into three granularities, and a point ratio is+2mm bulky grains, particle and -0.5mm little particles in+0.5mm~-2mm, wherein big
Grain returns to copper metallurgy industry；Middle particle carries out magnetic separation, magnetic field intensity 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 are 200 mesh；- 200 mesh materials that detailed catalogue is classified to obtain carry out high intensity magnetic separation using 16000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material returns to 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 focuses on；Copper powder is added according to chlorated liquid volume and enters line replacement, adds 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 and neutralized,
It is 6 to neutralize pH, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid and carries out acidolysis, finally controls pH
For 2.5, acidolysis slag and acid hydrolysis solution are filtrated to get, acidolysis slag returns to chloride process；Acid hydrolysis solution carries out extraction back extraction, and raffinate returns
Hydrolysis procedure, back extraction obtain copper sulphate and carry out electrodeposition, obtain electro deposited copper；Neutralize in the heavy copper liquid that heavy copper obtains and add bicarbonate
Sodium, adjustment pH=9 carry out heavy zinc, obtain heavy cadmia and heavy zinc liquid, and heavy cadmia cleans to obtain crude zinc and cleaning fluid, cleaning fluid and heavy
Zinc liquid returns to chloride process.Your slag gold content 12184g/t, silver content 135431g/t, palladium content 17880g/t.
Embodiment 3
Be 6.56% by copper content, Zn content 15.26%, gold content 23.50g/t, silver content 168.38g/t,
The anode furnace clinker that palladium content is 11.20g/t slightly break and sieve, slightly broken to use jaw crusher or kibbler roll,
Screening is divided into three granularities, and a point ratio is+2mm bulky grains, particle and -0.5mm little particles in+0.5mm~-2mm, wherein big
Grain returns to copper metallurgy industry；Middle particle carries out magnetic separation, magnetic field intensity 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 are 200 mesh；- 200 mesh materials that detailed catalogue is classified to obtain carry out high intensity magnetic separation using 12000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material returns to 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 focuses on；Copper powder is added according to chlorated liquid volume and enters line replacement, is added
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 and entered
Row neutralizes, and it is 5.5 to neutralize pH, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid and carries out acidolysis, most
It is 2 to control pH eventually, is filtrated to get acidolysis slag and acid hydrolysis solution, and acidolysis slag returns to chloride process；Acid hydrolysis solution carries out extraction back extraction, raffinate
Liquid returns to hydrolysis procedure, and back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；Neutralize in the heavy copper liquid that heavy copper obtains and add carbon
Sour hydrogen sodium, adjustment pH=8.5 carry out heavy zinc, obtain heavy cadmia and heavy zinc liquid, heavy cadmia and clean to obtain crude zinc and cleaning fluid, clean
Liquid and heavy zinc liquid return to chloride process.Your slag gold content 17357g/t, silver content 140087g/t, palladium content 12006g/t.
Embodiment 4
Be 5.06% by copper content, Zn content 18.99%, gold content 16.92g/t, silver content 180.18g/t,
The anode furnace clinker that palladium content is 22.84g/t slightly break and sieve, slightly broken to use jaw crusher or kibbler roll,
Screening is divided into three granularities, and a point ratio is+2mm bulky grains, particle and -0.5mm little particles in+0.5mm~-2mm, wherein big
Grain returns to copper metallurgy industry；Middle particle carries out magnetic separation, magnetic field intensity 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 are 200 mesh；- 200 mesh materials that detailed catalogue is classified to obtain carry out high intensity magnetic separation using 14000Gs magnetic separators, obtain
To magnetisable material and namagnetic substance, magnetisable material returns to 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 focuses on；Copper powder is added according to chlorated liquid volume and enters line replacement, is added
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
Neutralized, it is 5.5 to neutralize pH, is filtrated to get heavy copper ashes and heavy copper liquid；Heavy copper ashes adds the 98% industrial concentrated sulfuric acid and carries out acidolysis,
It is 2 finally to control pH, is filtrated to get acidolysis slag and acid hydrolysis solution, and acidolysis slag returns to chloride process；Acid hydrolysis solution carries out extraction back extraction, extraction
Extraction raffinate returns to hydrolysis procedure, and back extraction obtains copper sulphate and carries out electrodeposition, obtains electro deposited copper；Neutralize and added in the heavy copper liquid that heavy copper obtains
Sodium acid carbonate, adjustment pH=8.8 carry out heavy zinc, obtain heavy cadmia and heavy zinc liquid, heavy cadmia and clean to obtain crude zinc and cleaning fluid, clearly
Washing lotion and heavy zinc liquid return to chloride process.Your slag gold content 15043g/t, silver content 148366g/t, palladium content 17403g/t.
Claims (1)
- A kind of 1. method of anode furnace comprehensive utilization of slag, it is characterised in that step is as follows：(1) thick broken screening：Anode furnace clinker slightly break and sieve, thick break uses jaw crusher or kibbler roll, Screening is divided into three granularities, and a point ratio is+2mm bulky grains, particle and -0.5mm little particles in+0.5mm~-2mm, wherein big Grain returns to 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 return to copper metallurgy industry；(3) fine grinding is classified：The little particle and step (2) that step (1) obtains obtain namagnetic substance and carry out fine grinding, and fine grinding uses gas Stream mill or Ball-stirring mill, partition size are 200 mesh；(4) high intensity magnetic separation：- 200 mesh materials are obtained into step (3) and carry out high intensity magnetic separation, magnetic field intensity is 10000~16000Gs, is obtained To magnetisable material and namagnetic substance, magnetisable material returns to copper metallurgy industry；(5) chlorination：The namagnetic substance obtained into step (3) carries out chlorination, obtains chlorated liquid and chloride slag, and chloride slag is concentrated Processing；(6) copper powder is replaced：Copper powder is added in the chlorated liquid obtained to step (5) and enters line replacement, it is 0.5~2g/ to add copper powder amount L, your slag and displaced liquid of the noble metal of palladium containing gold and silver be filtrated to get；(7) heavy copper is neutralized：The displaced liquid obtained to step (6) adds sodium acid carbonate and neutralized, and it is 5~6 to neutralize pH, filtering Obtain heavy copper ashes and heavy copper liquid；(8) acidolysis：The heavy copper ashes obtained to step (7) adds sulfuric acid and carries out acidolysis, and it is 1.5~2.5 finally to control pH, is filtered To acidolysis slag and acid hydrolysis solution, acidolysis slag returns to 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 to acidolysis work Sequence, back extraction obtain copper sulphate and carry out electrodeposition, obtain electro deposited copper；(10) heavy zinc is neutralized：Sodium acid carbonate is added in the heavy copper liquid obtained to step (7), adjustment pH=8~9 carry out heavy zinc, obtained To heavy cadmia and heavy zinc liquid, heavy cadmia cleans to obtain crude zinc and cleaning fluid, and cleaning fluid and heavy zinc liquid return to chloride process；Chlorination uses sodium chloride, sodium chlorate and hydrochloric acid system in step (5), and sodium chloride concentration is 200~300g/L in system, chlorine Sour sodium addition is 20~30g/L, and 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 Hour, hydrochloric acid control solution pH=0.5~1 is used all the time in course of reaction.
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| 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 |
| 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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| JP3625270B2 (en) * | 2000-07-06 | 2005-03-02 | 太平洋セメント株式会社 | Waste disposal method |
| CL2014000785A1 (en) * | 2014-03-28 | 2016-01-29 | Alacran Spa | Process to recover copper, molybdenum and other metals from smelting slag |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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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