CN101775502A - Process for extracting copper from zinc hydrometallurgy flow - Google Patents

Process for extracting copper from zinc hydrometallurgy flow Download PDF

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Publication number
CN101775502A
CN101775502A CN201019144001A CN201019144001A CN101775502A CN 101775502 A CN101775502 A CN 101775502A CN 201019144001 A CN201019144001 A CN 201019144001A CN 201019144001 A CN201019144001 A CN 201019144001A CN 101775502 A CN101775502 A CN 101775502A
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Prior art keywords
copper
zinc
liquid
neutralization
deironing
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CN201019144001A
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Inventor
蒋绍平
朱国邦
鲁焘
姚斯吉
单祖宇
朱家华
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Yunnan Lancang Lead Ore Co Ltd
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Yunnan Lancang Lead Ore Co Ltd
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Priority to CN201019144001A priority Critical patent/CN101775502A/en
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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Abstract

The invention relates to a process for extracting copper from a zinc hydrometallurgy flow. In a wet flow of treating zinc oxide concentrate or zinc sulfide concentrate, two steps of preneutralization and copper extraction are added before a step of neutralization deferrization; the technical condition of the preneutralization is controlled accurately, so that copper ions are reserved in pre-neutralizing liquid, and then 80 percent of copper ions are deposited to copper concentrate by a zinc powder displacement method; the obtained copper concentrate contains 30 to 60 percent of copper and has great commercial value; and 20 percent of copper ions remained in the solution after displacement and copper extraction enter purifying residue through the steps of neutralization deferrization and purification, and then the copper ions are further subjected to enrichment in the purifying residue by the conventional method. In the process, 80 percent of the copper ions in leachate are extracted before the conventional steps of the purification and the neutralization deferrization; and by the recovery at the two stages, the recovery rate of the copper can reach over 80 percent.

Description

Process for extracting copper from zinc hydrometallurgy flow
Technical field:
The present invention relates to the non-ferrous metal metallurgy technical field, especially relate to a kind of technology that reclaims copper from flowsheet of wet zinc smelting.
Background technology:
At present, the wet process of handling zinc oxide concentrate by acidity leach, in and technologies such as deironing, purification, electrolysis constitute; The wet process of handling zinc sulfide concentrates by two sections oxygen press leach, in and deironing, purification, electrolysis process constitute.Generally speaking, the exhausted most infusion solution that in leaching process, enters of the copper in above-mentioned two kinds of technical process, and in and during most hydrolysis enters in the iron removal and in the iron barium slag after the deironing, cause the not recyclable loss of copper, rate of loss 70～80%.In and after the deironing in the liquid remaining cupric ion then when purifying, become metal with zinc dust precipitation, from solution, precipitate in the purification slag, will contain the lower purification slag of copper grade again and carry out the processing of enrichment slag to obtain copper ashes raw material and the Spongy Cadmium that grade is higher and have commodity value.
Summary of the invention:
The object of the present invention is to provide a kind of process for extracting copper from zinc hydrometallurgy flow, it in the wet process of handling zinc oxide concentrate or zinc sulfide concentrates, the wet process of handling zinc oxide concentrate comprise acidly leach, in and steps such as deironing, purification and electrolysis; The wet process of handling zinc sulfide concentrates comprise two sections oxygen press leach, in and steps such as deironing, purification, electrolysis, in and set up pre-neutralization before the deironing step and extract two steps of copper, the technical qualification of control pre-neutralization, cupric ion is retained in the pre-neutralization liquid, by zinc replacement 80% cupric ion is deposited in the copper ore concentrates again; By in existing and deironing, purification and electrolysis step extract 20% cupric ion in the liquid, further enriching and recovering behind the copper.
The extraction process for copper that the present invention proposes, the purification of routine and in and before the deironing step just with leach liquor in 80% cupric ion extract; Through two sections recovery, the rate of recovery of copper can reach more than 80%.
The present invention can be used for handling the zinc hydrometallurgy enterprise that raw material contains copper grade 〉=0.5% or leach liquor cupric 〉=500mg/L, and this technology can be strengthened zinc hydrometallurgy enterprise and comprehensively reclaim ability, improves the economic benefit that byproduct copper reclaims.
Each processing step cardinal principle of the present invention and technical qualification are as follows:
(1) two section oxygen is pressed and leached: this step is directly carried out selectivity to zinc sulfide concentrates and is leached under pressurization, logical oxygen and the condition of heating, and zinc sulphide and oxygen, waste electrolyte and sulfuric acid reaction generate vitriol, and elementary sulfur and water, cupric sulfide are also leached equally.Reaction formula is as follows:
ZnS+H 2SO 4+1/2O 2→ZnSO 4+H 2O+S
CuS+H 2SO 4+1/2O 2→CuSO 4+H 2O+S
Iron exists with the nZnS.mFeS form, presses in the leaching process at oxygen and is leached by selectivity, and reaction formula is as follows:
FeS+H 2SO 4+1/2O 2→FeSO 4+H 2O+S
2FeSO 4+H 2SO 4+1/2O 2→Fe 2(SO 4) 3+H 2O
ZnS+Fe 2(SO 4) 3→ZnSO 4+2FeSO 4+S
Fall when causing 3g/L when leaching acidity, iron generates siderotil and enters in the slag.
Oxygen is pressed the leaching-out technique condition:
Liquid-solid ratio: 5～7: 1, time: 60～90min, temperature: 140～150 ℃,
Oxygen partial pressure: 0.7～1.5Mpa, oxygen purity: 〉=99.6%,
Two sections leach liquors: contain acid～30g/L, iron content 8～10g/L;
One section leach liquor: contain acid 3～5g/L, iron content 2～3g/L contains zinc 120～160g/L, cupric 500～2000mg/L.
(2) the acid leaching:
ZnO in the zinc oxide concentrate, CuO, FeO and waste electrolyte and sulfuric acid carry out chemical reaction, generate the sulfate solution that contains things such as zinc, copper, iron.Reaction formula is as follows:
ZnO+H 2SO 4→ZnSO 4+H 2O
CuO+H 2SO 4→CuSO 4+H 2O
FeO+H 2SO 4→FeSO 4+H 2O
Fe 2O 3When peracid, partly dissolve: Fe 2O 3+ 3H 2SO 4→ Fe 2(SO 4) 3+ 3H 2O
Technical qualification:
Temperature: 70～80 ℃, liquid-solid ratio 5～7: 1, beginning acid: 120～150g/L,
Acid eventually: 0.5～5.0g/L, time: 40～60min/ jar.
(3) pre-neutralization:
In leach liquor, add neutralizing agent milk of lime (Ca (OH) 2) improve the pH value of solution, and be controlled at pH4.0～4.5 accurately; According to various metallic salt hydrolysis pH values, when ferric iron concentration was 2.0g/L, beginning hydrolysis pH was 1.7, and this moment, the ferric ion hydrolysis generated ferric hydroxide precipitate, and when copper ion concentration was 0.5g/L, the pH of beginning hydrolysis was 5.0; Thereby 90% or higher cupric ion be retained in the extraction process for copper that enters next step in the solution.Reaction formula is as follows:
H 2SO 4+Ca(OH) 2→CaSO 4↓+2H 2O
Fe 2(SO 4) 3+6H 2O→Fe(OH) 3↓+3H 2SO 4
Technical qualification:
Beginning acid: 0.5～7.0g/L, acid eventually: pH4.0～4.5, the time: 15～30min/ jar, temperature: 60～70 ℃, pressing filtering liquid solid content≤1.0mg/L, back liquid contains ferric iron≤100mg/L, back liquid cupric 500～2000mg/L
(4) extract copper:
Pre-neutralization liquid makes melt cinder separate after filtration, guarantees that filtered liquid is limpid, and analyzes and calculate the solution copper content.This filtered liquid extracts copper with zinc replacement, and the zinc powder add-on is by mass for carrying 80% of liquid copper metal amount before the copper.The principle that replacement(metathesis)reaction can be carried out is: based on the standard potential difference of various metals, promptly the metal that standard potential is lower can displace the higher metal of standard potential from solution.During 25 ℃ of temperature, zinc, cadmium, copper, standard potential be-0.762 volt ,-0.407 volt ,+0.345 volt.Given this principle, the replaceable cadmium of zinc, copper.
Reaction formula is as follows:
CuSO 4+Zn→ZnSO 4+Cu↓①
CdSO 4+Zn→ZnSO 4+Cd↓②
CuSO 4+Cd→CdSO 4+Cu↓③
The zinc powder add-on is 80% of a solution copper metal amount only, and the standard potential difference of zinc and copper is bigger, thereby only carries out 1. reaction formula in the process, 2. 3. reaction formula carries out hardly, cadmium is all stayed in the solution like this, and the zinc in the zinc powder all enters in the solution, has guaranteed the grade of displacement back copper ashes.
The zinc powder that uses in the extraction copper process can all enter solution, becomes liquid zinc, separates out to become zinc metal sheet when electrolysis, therefore can calculate at the mid-zinc powder cost of using instead of benefit calculation.
Technical qualification:
Beginning acid: pH4.0～4.5, acid eventually: pH5.2～5.4, the time: 10～20min/ jar,
Temperature: 60～65 ℃, the zinc powder add-on: carry before the copper in the solution 80% of copper metal amount,
The copper ore concentrates cupric: 30～60%, back liquid cupric: 100～200mg/L.
(5) in and deironing:
Through remove ferric iron and most cupric ion carry copper after liquid heat up, blowing air or pure oxygen add milk of lime once more and neutralize and remove two valency iron.Its principle is under the condition of pH5.2～5.4, utilizes airborne oxygen or pure oxygen that two valency iron in the solution are oxidized to goethite precipitation.Reaction formula is as follows:
2FeSO 4+1/2O 2+3H 2O→2FeOOH↓+2H 2SO 4
H 2SO 4+Ca(OH) 2→CaSO 4↓+2H 2O
Other has partly that two valency iron and arsenus acid, antimonous acid are oxidized to high price, and the ferric iron hydrolysis generates the colloid of lotus positive electricity, and the complex anion co-precipitation that absorption high price arsenic, antimony, germanium disassociation generate enters slag mutually and separated removing.Reaction formula is as follows:
Oxidation: 2FeSO 4+ 1/2O 2+ H 2SO 4→ Fe 2(SO 4) 3+ H 2O
HAsO 2+1/2O 2+H 2O→H 3AsO 4
HsbO 2+1/2O 2+H 2O→H 3SbO 4
Hydrolysis and disassociation:
Fe 2(SO 4) 3+6H 2O→2Fe(OH) 3↓+3H 2SO 4
Fe 2(SO 4) 3→2Fe 3++3(SO 4) 2-
H 3AsO 4→3H ++AsO 4 3-
H 3SbO 4→3H ++SbO 4 3-
H 2GeO 3→2H ++GeO 3 2-
Sorption-coprecipitation:
Fe (OH) 3Absorption Fe 3+→ Fe (OH) 3Fe 3+
xFe(OH) 3·yH 2O·ZFe 3+·AsO 4 3-↓
xFe(OH) 3·yH 2O·ZFe 3+·SbO 4 3-↓
xFe(OH) 3·yH 2O·ZFe 3+·GeO 3 2-↓
Technical qualification:
Whole sour pH5.2～5.4,70～80 ℃ of temperature, time 1～4h/ jar,
Liquid iron content≤10mg/L after the deironing, arsenic≤0.2mg/L, antimony≤0.2mg/L, germanium≤0.1mg/L.Through in and solution after the deironing remove impurity such as whole cadmiums and remaining copper, germanium, cobalt, nickel again to purifying step, obtain purified new liquid and send to electrolysis with production metal zinc metal sheet.
The purification slag of purifying step output carries out the copper ashes that enrichment for the second time obtains commodity value with traditional technology again, simultaneously the output Spongy Cadmium.Through this twice recovery, the rate of recovery of copper just can reach more than 80%.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
The present invention is further described below in conjunction with process flow sheet:
Embodiment:
Embodiment 1:
Billows deep blue lead ore company limited zinc smeltery, Yunnan adopts two sections oxygen to press and leaches flow process, and it is as follows to extract the process for copper situation with the invention process:
(1) two section oxygen is pressed and is leached:
Temperature is 140～150 ℃ in the autoclave, oxygen partial pressure 0.8～1.4MPa, and liquid-solid ratio 5～7: 1, time 60～90min;
One section leach liquor composition: Zn153.84g/L, H +6.18g/L, ∑ Fe4.59g/L, Fe 2+3.45g/L, Cu1628.79mg/L, Cd1124.6mg/L, As824.47mg/L, Sb21.09mg/L, Ge0.66mg/L, Co7.24mg/L, Ni3.27mg/L.
(2) pre-neutralization:
The sour 6.18g/L that begins, 60～65 ℃ of temperature, sour pH4.2～4.4 eventually, time 20min/ jar, neutralizing agent milk of lime.
Liquid after the pre-neutralization: Zn148.72g/L, ∑ Fe3.35g/L, Fe 2+3.11g/L, Cu1570.62mg/L, speed of filter pressing 7.5L/m 2Min, pressing filtering liquid solid content 0.8mg/L, cupric ion retention rate 96.43%.
(3) extract copper:
60～65 ℃ of temperature, time 15min/ jar is carried preceding liquid: the Zn151.28g/L of copper, ∑ Fe3.37g/L, Fe 2+3.24g/L, Cu1633.66mg/L, Cd1010.64mg/L.
The zinc powder add-on is to carry 80% of the preceding liquid copper metal amount of copper, and preceding liquid amasss 42m 3, preceding liquid copper metal amount: 42m 3* 1633.66g/m 3=68.6kg.
Zinc powder purity 83%, zinc powder add-on: (68.6 ÷ 83%) * 80%=66.12kg.
Carry liquid: Zn162.17g/L behind the copper, ∑ Fe3.47g/L, Cu104.76mg/L, Cd980.88mg/L.
Copper extraction yield (1633.66-104.76)/1633.66 * 100%=93.59%, copper ore concentrates grade are 57.08%.
(4) in and deironing:
72～75 ℃ of temperature, whole sour pH5.2～5.4, time 2.5h/ jar, neutralizing agent milk of lime.
Liquid Zn158.06g/L after the deironing, ∑ Fe6.6m g/L, Cu88.04mg/L, Cd966.08mg/L, As0.07mg/L, Sb1.07mg/L, Ge0.054mg/L.
Through in and solution after the deironing arrive again purify and electrolysis step with traditional technology production metal zinc metal sheet.
Embodiment 2:
Be all two sections oxygen and press the leaching flow process, extract process for copper with the invention process, parameter is as follows:
The condition that leaches is with (1) among the embodiment 1;
One section leach liquor composition: Zn160.82g/L, H +4.82g/L, ∑ Fe2.88g/L, Fe 2+1.62g/L, Cu1927.2mg/L, Cd1620.6mg/L, As726.24mg/L, Sb18.06mg/L, Ge0.81mg/L, Co5.74mg/L, Ni1.57mg/L.
(2) pre-neutralization:
The sour 4.82g/L that begins, 60～65 ℃ of temperature, sour pH4.2～4.4 eventually, time 18min/ jar, neutralizing agent milk of lime.
Liquid after the pre-neutralization: Zn154.61g/L, ∑ Fe1.8g/L, Fe 2+1.58g/L, Cu1680.48mg/L, Cd1544.2mg/L, speed of filter pressing 8.0L/m 2Min, pressing filtering liquid solid content 1.0mg/L, cupric ion retention rate 87.20%.
(3) extract copper:
60～65 ℃ of temperature, time 15min/ jar, the zinc powder add-on is to carry 80% of the preceding liquid copper metal amount of copper, speed of filter pressing: 10.4L/min carries preceding liquid: the Zn154.61g/L of copper, ∑ Fe1.80g/L, Fe 2+1.58g/L, Cu1680.48mg/L, Cd1544.2mg/L.
The long-pending 42m of preceding liquid 3, preceding liquid copper metal amount: 42m 3* 1680.48g/m 3=70.58kg.
Zinc powder purity 83%, zinc powder add-on: (70.58 ÷ 83%) * 80%=68.03kg.
Carry liquid: Zn161.88g/L behind the copper, ∑ Fe1.8g/L, Cu162.46mg/L, Cd1481.2mg/L.
Copper extraction yield (1680.48-162.46)/1680.48 * 100%=90.33%, copper ore concentrates grade are 54.87%.
(4) in and deironing:
70～75 ℃ of temperature, whole sour pH5.2～5.4, time 1.8h/ jar, neutralizing agent milk of lime.
Liquid Zn155.66g/L after the deironing, ∑ Fe4.2mg/L, Cu60.4mg/L, Cd1366.2mg/L, As0.045mg/L, Sb2.02mg/L, Ge0.062mg/L.
Through in and deironing after the solution subsequent disposal with embodiment 1.

Claims (3)

1. process for extracting copper from zinc hydrometallurgy flow, the wet process of handling zinc oxide concentrate comprise acidly leach, in and deironing, purification and electrolysis step; The wet process of handling zinc sulfide concentrates comprise two sections oxygen press leach, in and deironing, purification, electrolysis step, it is characterized in that: in and set up pre-neutralization before the deironing step and extract two steps of copper, the technical qualification of control pre-neutralization, cupric ion is retained in the pre-neutralization liquid, by zinc replacement 80% cupric ion is deposited in the copper ore concentrates again; By in existing and deironing, purification and electrolysis step extract 20% cupric ion in the liquid, further enriching and recovering behind the copper.
2. extraction process for copper according to claim 1 is characterized in that said pre-neutralization step technique condition is:
Beginning acid: 0.5～7.0g/L, acid eventually: pH4.0～4.5, the time: 15～30min/ jar, temperature: 60～70 ℃, pressing filtering liquid solid content≤1.0mg/L, back liquid contains ferric iron≤100mg/L, back liquid cupric 500～2000mg/L.
3. extraction process for copper according to claim 1 is characterized in that said extraction copper step technique condition is:
Beginning acid: pH4.0～4.5, acid eventually: pH5.2～5.4, the time: 10～20min/ jar, temperature: 60～65 ℃, the zinc powder add-on is by mass for carrying 80% of liquid copper metal amount before the copper, carries liquid cupric: 100～200mg/L behind the copper.
CN201019144001A 2010-02-04 2010-02-04 Process for extracting copper from zinc hydrometallurgy flow Pending CN101775502A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010995A (en) * 2010-12-29 2011-04-13 株洲冶炼集团股份有限公司 Method for increasing copper recovery rate in zinc hydrometallurgy process
CN102676815A (en) * 2012-06-08 2012-09-19 大兴安岭云冶矿业开发有限公司 Method for removing iron from leach liquor at two stages
CN103667720A (en) * 2013-12-26 2014-03-26 河南豫光锌业有限公司 Method for recovering zinc, indium, iron, and lead from high-iron zinc oxide mixture smelted with zinc
CN108624910A (en) * 2018-04-16 2018-10-09 北京科技大学 A kind of zinc Whote-wet method smelting process method of energy-saving and emission-reduction
CN108913893A (en) * 2018-07-29 2018-11-30 桂林理工大学 A kind of zinc hydrometallurgy zinc powder consumption-reducing method
WO2020062145A1 (en) * 2018-09-29 2020-04-02 长沙有色冶金设计研究院有限公司 Oxygen pressure leaching method for copper sulfide concentrate and copper smelting method
CN112501452A (en) * 2020-11-05 2021-03-16 矿冶科技集团有限公司 Method for purifying zinc mineral material leaching solution

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010995A (en) * 2010-12-29 2011-04-13 株洲冶炼集团股份有限公司 Method for increasing copper recovery rate in zinc hydrometallurgy process
CN102676815A (en) * 2012-06-08 2012-09-19 大兴安岭云冶矿业开发有限公司 Method for removing iron from leach liquor at two stages
CN103667720A (en) * 2013-12-26 2014-03-26 河南豫光锌业有限公司 Method for recovering zinc, indium, iron, and lead from high-iron zinc oxide mixture smelted with zinc
CN103667720B (en) * 2013-12-26 2015-07-22 河南豫光锌业有限公司 Method for recovering zinc, indium, iron, and lead from high-iron zinc oxide mixture smelted with zinc
CN108624910A (en) * 2018-04-16 2018-10-09 北京科技大学 A kind of zinc Whote-wet method smelting process method of energy-saving and emission-reduction
CN108913893A (en) * 2018-07-29 2018-11-30 桂林理工大学 A kind of zinc hydrometallurgy zinc powder consumption-reducing method
CN108913893B (en) * 2018-07-29 2020-04-14 桂林理工大学 Zinc powder consumption reduction method for zinc hydrometallurgy
WO2020062145A1 (en) * 2018-09-29 2020-04-02 长沙有色冶金设计研究院有限公司 Oxygen pressure leaching method for copper sulfide concentrate and copper smelting method
CN112501452A (en) * 2020-11-05 2021-03-16 矿冶科技集团有限公司 Method for purifying zinc mineral material leaching solution

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Application publication date: 20100714