CN108034830B - A kind of method of valuable metal in Recovering Copper smelting ash - Google Patents

A kind of method of valuable metal in Recovering Copper smelting ash Download PDF

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CN108034830B
CN108034830B CN201711413502.7A CN201711413502A CN108034830B CN 108034830 B CN108034830 B CN 108034830B CN 201711413502 A CN201711413502 A CN 201711413502A CN 108034830 B CN108034830 B CN 108034830B
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copper
cigarette ash
iron
sulfuric acid
low
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CN108034830A (en
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汪金良
胡华舟
谢凌峰
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Jiangxi Shanning Technology Co ltd
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Jiangxi University of Science and Technology
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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
    • C22B7/02—Working-up flue dust
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00—Magnetic separation
    • B03C1/02—Magnetic separation acting directly on the substance being separated
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • 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
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0065—Leaching or slurrying
    • C22B15/0067—Leaching or slurrying with acids or salts thereof
    • C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/04—Obtaining arsenic
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/06—Obtaining bismuth
    • 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
    • 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 of valuable metal in Recovering Copper smelting ash, and Copper making cigarette ash initial gross separation is obtained rich iron cigarette ash and low iron cigarette ash using magnetic selection method first；Rich iron cigarette ash obtains rich scum and copper-bath through sulfuric acid leaching；Low iron cigarette ash obtains middle phase analysis and middle immersion liquid through neutrality leaching；Middle phase analysis through low acid solution leach neutral leaching is returned in high lead bismuth slag and pickle liquor, pickle liquor；Middle immersion liquid is through SO2Restore to obtain As2O3And copper-bath, copper-bath carry out electrodeposition and obtain fine copper.The present invention uses magnetic separation separation and culture method, and the atrament containing a large amount of iron and a small amount of copper of cigarette ash total amount about 20% is separated, reduces neutral leaching process amount, the content of immersion liquid arsenic, facilitates SO in raising2Heavy arsenic is restored, while reducing the influence that iron filters acidleach, the acidity of acidleach can be greatly improved, arsenic content in acid leaching residue is reduced, obtains rich scum, high lead bismuth slag and high purity copper, realize the synthetical recovery of valuable metal.

Description

A kind of method of valuable metal in Recovering Copper smelting ash
Technical field
The present invention relates to a kind of integrated conduct method of nonferrous metallurgical process solid waste, especially selecting smelting combinations from copper smelting The method for refining comprehensively recovering valuable metal in cigarette ash.
Background technique
Contain a variety of valuable metals such as Cu, Fe, As, Pb, Zn, Bi, grade in a large amount of cigarette ashes generated during Copper making Higher than general ore, there is very high comprehensive utilization value, the comprehensive reutilization of valuable metal is constantly subjected to extensive concern. Common method has alkaline leaching, acidic leaching and the wet method combined method of pyrogenic process etc..
Since during Copper making, most of cigarette ashes return to smelting system, outlet is just considered as Pb, As higher, therefore Outer discharge capacity is smaller, is suitble to wet processing process.It is wherein most widely used with sulfuric acid leaching, Hou Xin is just equal (from copper converter cigarette Copper, zinc experimental study hydrometallurgy, 2011,30 (1): 57-59. are leached in ash) sulfuric acid leaching ash of copper converter is used, 1.80 mol/L of sulfuric acid concentration, liquid-solid ratio 7:1,1.5 h are leached under the conditions of 70 DEG C of extraction temperature, the leaching rate of Cu, Zn are up to 90 % or more, Fe, Pb then enter in slag, and the method simple process, environmental pollution are small conducive to environmental protection；The disadvantage is that liquid-solid ratio is excessive, leaches Liquid metal concentration is low and Pb and Fe do not obtain further separation and concentration.(Copper smelting dust sulfuric acid leaching and copper are leached and are moved Sun Ledong etc. Mechanics study mining metallurgical engineering, 2016,36 (1): 97-100.) have studied the power credit of sulfuric acid leaching Copper smelting dust process Analysis, the results showed that sulfuric acid leaching process belongs to diffusion control, and the apparent activation energy of Leach reaction Cu is 8.05 kJ/mol, therefore can Reinforce diffusion control effect by improving the means such as liquid-solid ratio, mixing speed.(copper in high arsenic white cigarette ash is soaked in roasting to Zhang Xiaofeng etc. The influence of extracting rate and its thermodynamic analysis mining metallurgical engineering, 2012,32 (5): 86-89.) have studied white cigarette ash roasting transition- Acidleach thermodynamics, the results showed that, roasting can convert ease of solubility copper for the copper sulfide of slightly solubility and cuprous oxide, greatly improve The leaching rate of copper explains the not high reason of copper leaching rate during direct acidleach, but roasts in transformation process that there are arsenic Vaporization behaviors are unfavorable for environmental protection.Patent application 200910080464.7,201410690393.3,201510693277.1, 201610030159.7 etc. disclose the method that sulfuric acid system leaches Bellamya aeruginosa, realize the leaching of good valuable element, But these method common ground are all that process flow is long, Steep cencentration is low, is also easy to produce " three wastes ".
Experimental study discovery, the atrament for being about 20% containing mass percent in Copper making cigarette ash, through assay, This substance contains a large amount of Armco magnetic irons and a small amount of copper, has stronger magnetism.For this purpose, the present invention using magnetic selection method to cigarette ash into Row pretreatment, isolates most of atrament, reduce it is neutral leach cigarette ash treating capacity, in raising in immersion liquid arsenic content, Facilitate SO2Heavy arsenic is restored, while reducing the influence that iron filters acidleach, the acidity of acidleach can be greatly improved, reduces acidleach Arsenic content in slag, and rich scum, high lead bismuth slag and high purity copper can be obtained, it realizes the synthetical recovery of valuable metal, there is technique Simply, the features such as selectivity is good, without " three wastes " discharge, economy and obvious environment benefit, has good promotional value.
Summary of the invention
In order to achieve the above objectives, it the present invention provides a kind of method of valuable metal in Recovering Copper smelting ash, adopts The technical solution taken is as follows.
Initial gross separation is carried out to Copper making cigarette ash using magnetic selection method, obtains rich iron cigarette ash and low iron cigarette ash；Rich iron cigarette ash Through sulfuric acid leaching, rich scum and copper-bath are obtained；Low iron cigarette ash obtains middle phase analysis and middle immersion liquid through neutrality leaching；Middle phase analysis Through dilute sulfuric acid leach neutral leaching is returned in high lead bismuth slag and pickle liquor, pickle liquor；Middle immersion liquid is through SO2Restore to obtain As2O3And copper sulphate Solution, copper-bath carry out electrodeposition and obtain fine copper, and liquid returns rich iron cigarette ash acidleach after electrodeposition.Specific technical process and technological parameter It is as follows.
A. magnetic separation.Copper making cigarette ash is subjected to magnetic separation separation under the magnetic induction intensity of 0.4-0.8T, obtains rich iron cigarette ash With low iron cigarette ash.
B. acidleach.Acidleach is carried out to rich iron cigarette ash using sulfuric acid, obtains rich scum and copper-bath.Acidleach condition are as follows: Sulfuric acid concentration is 1-5mo/L, and the liquid-solid ratio of sulfuric acid and Fu Tie cigarette ash is 1:1-6:1 mL/g, and temperature is 45-85 DEG C, and the time is 0.5-2.0 h。
C. neutral to leach.Neutral leaching is carried out to low iron cigarette ash using dilute sulfuric acid, obtains neutral phase analysis and neutral immersion liquid.In Property leaching condition are as follows: dilute sulfuric acid concentration is 0.1-0.5mol/L, and the liquid-solid ratio of dilute sulfuric acid and low iron cigarette ash is 1:1-6:1 mL/g, Temperature is 25-45 DEG C, and the time is 0.5-2.0 h.
D. heavy arsenic is restored.Neutral immersion liquid is subjected to SO2Heavy arsenic is restored, As is obtained2O3And copper-bath.Restore heavy arsenic item Part are as follows: SO2Intake is 1-5 times of theoretical amount, and temperature is 45-85 DEG C, and the time is 0.5-2.0 h.
E. Weak-acid leaching.Neutral phase analysis is leached using low acid solution, obtains high lead bismuth slag and low pickle liquor.Low acidleach Condition out are as follows: sulfuric acid concentration is 0.1-0.5mo/L in low acid solution, and the liquid-solid ratio of low acid solution and neutral phase analysis is 1:1-5:1 mL/ G, temperature are 45-85 DEG C, and the time is 0.5-2.0 h.
F. electrodeposition.The copper-bath that step b, d is obtained carries out conventional copper electrodeposition, after obtaining cathode fine copper and electrodeposition Liquid, liquid returns rich iron cigarette ash acidleach after electrodeposition.
Further, the Copper making cigarette ash iron content 5-30wt.%, cupric 1-40wt.%, 5-25wt.% containing arsenic, leaded 5- 25wt.%, bismuth-containing 1-10wt.%.
Further, the mixing speed reacted in described step b, c, d, e is 200-400 r/min.
Further, the SO in the step d2Flow is 0.5-2.0 L/min.
Further, the low pickle liquor in the step e returns to low iron cigarette ash neutrality and leaches, and high lead bismuth slag can send lead to smelt System；Liquid returns to rich iron cigarette ash acidleach after electrodeposition in the step f.
Compared with Copper making cigarette ash resource utilization existing method, the invention has the advantages that.
(1) the pretreated method of magnetic separation is used, by the black object containing most of iron and part copper of 20 % of cigarette ash total amount Matter is separated, and iron is individually recycled.
(2) neutral leaching cigarette ash treating capacity is reduced, the concentration of immersion liquid arsenic, facilitates SO in raising2Restore heavy arsenic.
(3) influence that iron filters acidleach is reduced, the acidity of acidleach can be greatly improved, reduce arsenic content in acid leaching residue.
(4) high lead bismuth slag can be obtained, be conducive to comprehensive recovery of lead and bismuth.
(5) high-concentration sulfuric acid copper solution can be obtained, be conducive to electrodeposition recycling high purity copper, or crystallization recycling copper sulphate.
Detailed description of the invention
Fig. 1: process flow chart of the invention schematic diagram.
Fig. 2: the XRD spectrum of experimental raw Copper making cigarette ash.
Fig. 3: the XRD spectrum of rich iron cigarette ash.
Fig. 4: the XRD spectrum of low iron cigarette ash.
Specific embodiment
Below with reference to embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than it is right Of the invention further limits.
Embodiment 1:
100g Copper making cigarette ash (wCu15.22%, wFe9.50%, wAs8.40%, wPb12.22%, wBi3.2%) in the magnetic of 0.55T Physical separation is carried out under induction, obtains rich iron cigarette ash 20.5g and low iron cigarette ash 79.5g；Rich iron cigarette ash through 2mol/L sulfuric acid, In liquid-solid ratio 3:1, temperature is 75 DEG C, time 1h, and revolving speed is 300r/min leaching, obtains rich scum and copper-bath；It is low Iron cigarette ash is through 0.05mol/L sulfuric acid, and in liquid-solid ratio 3:1, temperature is 75 DEG C, time 1h, and revolving speed is 300r/min leaching, obtains Middle phase analysis and middle immersion liquid；Middle phase analysis is through 0.2 mol/L sulfuric acid, and in liquid-solid ratio 3:1, temperature is 75 DEG C, time 1h, and revolving speed is 300r/min is leached, and obtains high lead bismuth slag and pickle liquor；Middle immersion liquid is through SO2Intake is 3 times of theoretical amount, SO2Flow is 1 L/min, temperature are 75 DEG C, time 1h, and revolving speed is that 300r/min restores heavy arsenic, obtain As2O3And copper-bath.With this On the basis of the content of each phase accounts for ratio of the element in material content, essential element is allocated as follows element in experiment.
Embodiment 2:
100g Copper making cigarette ash (wCu15.22%, wFe9.50%, wAs8.40%, wPb12.22%, wBi3.2%) in the magnetic of 0.4T Physical separation is carried out under induction, obtains rich iron cigarette ash 23.6g and low iron cigarette ash 76.4g；Rich iron cigarette ash through 2mol/L sulfuric acid, In liquid-solid ratio 4:1, temperature is 85 DEG C, time 1h, and revolving speed is 300r/min leaching, obtains rich scum and copper-bath；It is low Iron cigarette ash is through 0.04mol/L sulfuric acid, and in liquid-solid ratio 4:1, temperature is 85 DEG C, time 1h, and revolving speed is 300r/min leaching, obtains Middle phase analysis and middle immersion liquid；Middle phase analysis is through 0.4 mol/L sulfuric acid, and in liquid-solid ratio 4:1, temperature is 85 DEG C, time 1h, and revolving speed is 300r/min is leached, and obtains high lead bismuth slag and pickle liquor；Middle immersion liquid is through SO2Intake is 1 times of theoretical amount, SO2Flow is 1 L/min, temperature are 85 DEG C, time 1h, and revolving speed is that 300r/min restores heavy arsenic, obtain As2O3And copper-bath.With this On the basis of the content of each phase accounts for ratio of the element in material content, essential element is allocated as follows element in experiment.
Embodiment 3:
100g Copper making cigarette ash (wCu15.22%, wFe9.50%, wAs8.40%, wPb12.22%, wBi3.2%) in the magnetic of 0.7T Physical separation is carried out under induction, obtains rich iron cigarette ash 22.8g and low iron cigarette ash 77.2g；Rich iron cigarette ash through 2mol/L sulfuric acid, In liquid-solid ratio 5:1, temperature is 85 DEG C, time 1h, and revolving speed is 400r/min leaching, obtains rich scum and copper-bath；It is low Iron cigarette ash is through 0.02mol/L sulfuric acid, and in liquid-solid ratio 5:1, temperature is 85 DEG C, time 1h, and revolving speed is 300r/min leaching, obtains Middle phase analysis and middle immersion liquid；Middle phase analysis is through 0.2 mol/L sulfuric acid, and in liquid-solid ratio 5:1, temperature is 85 DEG C, time 1h, and revolving speed is 400r/min is leached, and obtains high lead bismuth slag and pickle liquor；Middle immersion liquid is through SO2Intake is 1 times of theoretical amount, SO2Flow is 5 L/min, temperature are 45 DEG C, time 2h, and revolving speed is that 400r/min restores heavy arsenic, obtain As2O3And copper-bath.With this On the basis of the content of each phase accounts for ratio of the element in material content, essential element is allocated as follows element in experiment.

Claims (4)

1. a kind of method of valuable metal in Recovering Copper smelting ash, which comprises the following steps:
A. magnetic separation
Copper making cigarette ash is subjected to magnetic separation separation under the magnetic induction intensity of 0.4-0.8T, obtains rich iron cigarette ash and low iron cigarette ash； The Copper making cigarette ash iron content 5-30wt.%, cupric 1-40wt.%, 5-25wt.% containing arsenic, leaded 5-25wt.%, bismuth-containing 1- 10wt.%；
B. acidleach
Acidleach is carried out to rich iron cigarette ash using sulfuric acid, obtains rich scum and copper-bath, acidleach condition are as follows: sulfuric acid concentration 1- The liquid-solid ratio of 5mo/L, sulfuric acid and Fu Tie cigarette ash is 1:1-6:1 mL/g, and temperature is 45-85 DEG C, and the time is 0.5-2.0 h；
C. neutral to leach
Neutral leaching is carried out to low iron cigarette ash using dilute sulfuric acid, obtains neutral phase analysis and neutral immersion liquid, neutral leaching condition are as follows: dilute Sulfuric acid concentration is 0.1-0.5mol/L, and the liquid-solid ratio of dilute sulfuric acid and low iron cigarette ash is 1:1-6:1 mL/g, and temperature is 25-45 DEG C, Time is 0.5-2.0 h；
D. heavy arsenic is restored
Neutral immersion liquid is subjected to SO2Heavy arsenic is restored, As is obtained2O3And copper-bath, restore heavy arsenic condition are as follows: SO2Intake is 1-5 times of theoretical amount, temperature are 45-85 DEG C, and the time is 0.5-2.0 h；
E. Weak-acid leaching
Neutral phase analysis is leached using low acid solution, obtains high lead bismuth slag and low pickle liquor, Weak-acid leaching condition are as follows: low acid solution Middle sulfuric acid concentration is 0.1-0.5mol/L, and the liquid-solid ratio of low acid solution and neutral phase analysis is 1:1-5:1 mL/g, temperature 45-85 DEG C, the time is 0.5-2.0 h；
F. electrodeposition
The copper-bath that step b, d is obtained carries out conventional copper electrodeposition, obtains liquid after cathode fine copper and electrodeposition.
2. the method according to claim 1, wherein the mixing speed reacted in described step b, c, d, e is 200-400 r/min。
3. the method according to claim 1, wherein the SO in the step d2Flow is 0.5-2.0 L/min.
4. the method according to claim 1, wherein the low pickle liquor in the step e returns in low iron cigarette ash Property leach, high lead bismuth slag send lead smelting system；Liquid returns to rich iron cigarette ash acidleach after electrodeposition in the step f.
CN201711413502.7A 2017-12-24 2017-12-24 A kind of method of valuable metal in Recovering Copper smelting ash Active CN108034830B (en)

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CN109182764A (en) * 2018-09-30 2019-01-11 昆明理工大学 A kind of soda acid joint clean method of Copper making flue dust synthetical recovery
CN114107680A (en) * 2021-10-22 2022-03-01 王进 Method for extracting valuable and rare metals from fly ash furnace gas in rock wool production

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US4244734A (en) * 1979-07-19 1981-01-13 Hazen Research, Inc. Process for recovering metal values from materials containing arsenic
JP4411057B2 (en) * 2003-11-28 2010-02-10 三井金属鉱業株式会社 Arsenic removal method from smoke ash
CN101037725A (en) * 2007-02-06 2007-09-19 朱永文 Method for treating arsenic pollution of copper smelt industry
CN103014355B (en) * 2012-12-13 2014-12-24 马永涛 Multi-metal comprehensive recycling process for copper smelting ash
CN104593604A (en) * 2015-01-09 2015-05-06 紫金矿业集团股份有限公司 Process of recovering copper smelting waste acid and white smoke dusts
CN106544513A (en) * 2016-11-09 2017-03-29 河南中原黄金冶炼厂有限责任公司 A kind of method of copper smelting by pyrometallurgy white cigarette dirt valuable metal recovery

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