CN101935761A - Method for separating copper, selenium and tellurium from lead matte - Google Patents

Method for separating copper, selenium and tellurium from lead matte Download PDF

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Publication number
CN101935761A
CN101935761A CN2010102435118A CN201010243511A CN101935761A CN 101935761 A CN101935761 A CN 101935761A CN 2010102435118 A CN2010102435118 A CN 2010102435118A CN 201010243511 A CN201010243511 A CN 201010243511A CN 101935761 A CN101935761 A CN 101935761A
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copper
lead
tellurium
sulfuric acid
leaching
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杨天足
文剑锋
蔡练兵
王安
肖峰
刘伟锋
窦爱春
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Central South University
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Central South University
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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 method for separating copper, selenium and tellurium from lead matte. The method comprises the following steps of: mixing smashed lead matte powder, sodium hydroxide, sodium carbonate and water by a certain proportion and putting an obtained mixture into a high-pressure kettle; introducing oxygen into the high-pressure kettle and controlling the pressure of the oxygen in the kettle to carry out an oxidation reaction, wherein selenium is oxidized into alkaline leaching liquor, and copper, lead and tellurium are oxidized into an alkaline leaching residue; and leaching the alkaline leaching residue by using a sulfuric acid solution to leach out the copper and the tellurium, wherein the lead is enriched in an acidic leaching residue. In the invention, the leaching rate of the copper reaches higher than 98 percent, and the leaching rate of the tellurium reaches higher than 90 percent. The invention has the advantages of low requirement on materials, small corrosion to equipment of alkaline media, safe operation, good comprehensive recovery benefit of valuable metals, low labor intensity, short treatment time and good operation environment.

Description

A kind of from lead copper matte the method for separating copper and selen-tellurjum
Technical field the present invention relates to hydrometallurgy process in the field of metallurgy, particularly the Wet-process metallurgy method of separating copper and selen-tellurjum effectively in the by product lead copper matte from plumbous smelting process.
Background technology lead copper matte (being commonly called as lead matte) is a kind of by product that mainly contains copper and plumbous sulfide of lead ore concentrate output in blast furnace smelting and oxygen bottom-blowing process, wherein enrichment the copper in the lead ore concentrate, selenium, tellurium, and contain the plumbous and silver-colored of some, be the important source material that reclaims copper, selenium, tellurium.At present, the processing of lead copper matte is that the raw material as copper metallurgy enters the copper smelting system, and promptly the higher lead copper matte of cupric directly carries out bessemerizing of copper, and plumbous and sulphur enters the gas phase volatilization, and the output blister copper carries out electrorefining, plumbous form recovery with flue dust; The lead copper matte that cupric is lower carries out the oxidizing roasting desulfurization, and copper changes into cupric oxide or copper sulfate, with sulfuric acid leaching copper is separated with lead, and the copper-bath of output enters the copper smelting system, and leached mud returns lead system.In recent years, studied and adopted the sulfuric acid pressure oxidation leaching-out method to carry out copper and plumbous separating, the copper-bath of output reclaims copper by electrodeposition, and leached mud returns plumbous smelting system.So and society, " the copper smelting technology " of work such as Li Mingzhao. the .2007.1 of Chemical Industry Press; Chinese patent application 200810058113.1 " reclaims the technology of copper " from lead matte.
There is following shortcoming in the treatment process of above-mentioned lead copper matte (lead matte):
(1) lead copper matte that copper content the is high system of bessemerizing that enters copper obtains blister copper, and plumbous voloxidation is entered gas phase separation, and technical process is long, and the rate of recovery of metal is low, the cost height, and the blister copper quality of output is low.The lead copper matte of plumbous smeltery output can only be sold to copper smelting plant as copper raw material, and the lead in the lead copper matte, silver, selenium, tellurium etc. are all without charge, and economic benefit is low.
(2) lead copper matte that copper content is lower is used the sulfuric acid leaching separating copper after handling with the oxidizing roasting method again, because the easy sintering of roasting process, the oxidation of cupric sulfide is not thorough, causes copper recovery low; Other valuable metals such as dispersions such as selenium, tellurium in the lead copper matte are difficult to reclaim; Process produces low concentration sulphur dioxide flue gas and pollutes.
(3) though the sulfuric acid pressure oxidation leaching-out method can be realized separating of copper and lead, but the selen-tellurjum in the lead copper matte disperses to be unfavorable for reclaiming, the equipment corrosion problem that acid leaching system of while exists inevitably, equipment corrosion speed is fast, the frequency of maintenance height, make acid pressure exerting device for a long time normal use in industrial production.
Summary of the invention the purpose of this invention is to provide a kind of oxidation of carrying out lead copper matte in alkaline medium, can realize separating of copper and lead effectively, and the selen-tellurjum in the enriching and recovering lead copper matte, and the free of contamination substantially Wet-process metallurgy method of process.
For the technical solution used in the present invention that achieves the above object is the lead copper matte powder after the fragmentation, sodium hydroxide, yellow soda ash, water to be mixed by certain proportioning drop into autoclave, at a certain temperature, aerating oxygen and the pressure of controlling oxygen in the still carry out oxidizing reaction in the autoclave, selenium is oxidized to enter alkaline leach liquor, copper, lead and tellurium be oxidized to enter alkaline leached mud, the alkalescence leached mud leaches copper and tellurium with sulphuric acid soln again, and lead is enriched in the acid leached mud.
Concrete treatment process is as follows:
1 oxidation is leached
Lead copper matte is earlier broken and wear into the powder that particle diameter is 0.25～0.074mm, and with certain density sodium hydroxide and sodium carbonate solution pulp and add in the autoclave, heating up afterwards, aerating oxygen carries out oxidizing reaction.The temperature of oxidizing reaction is 150～250 ℃, naoh concentration is 1.0～3.0mol/L, concentration of sodium carbonate is 0～2mol/L, the weight liquid-solid ratio that the leaches ratio of lead copper matte weight (solution weight with) is 3～10: 1, the dividing potential drop of oxygen is controlled at 0.3～1.5MPa, the total pressure of system maintains 1.5～3.5MPa, and the reaction times is 2～6h.After reaction finishes, be cooled to 20～60 ℃, filter.The main chemical reactions that the oxidation leaching process takes place is:
Cu 2S+2.5O 2+2NaOH+H 2O＝2Cu(OH) 2↓+Na 2SO 4 (1)
Cu 2S+2.5O 2+2Na 2CO 3+H 2O＝2CuCO 3↓+Na 2SO 4+2NaOH (2)
PbS+2O 2＝PbSO 4↓ (3)
PbS+2O 2+2NaOH＝Pb(OH) 2↓+Na 2SO 4 (4)
PbS+2O 2+Na 2CO 3＝PbCO 3↓+Na 2SO 4 (5)
Cu 2Se+2O 2+2NaOH+H 2O＝2Cu(OH) 2+Na 2SeO 3 (6)
Cu 2Te+2.5O 2+2NaOH+H 2O＝2Cu(OH) 2+Na 2TeO 4↓ (7)
The sulfuric acid that 2 alkali soak slag leaches
The leached mud that obtains after the reaction is leached in oxidation, is under 70～85 ℃ in temperature, is that the sulphuric acid soln of 0.5～2.5mol/L is 2～8: 1 with the weight liquid-solid ratio with concentration, leach 2～3h, after sulfuric acid leaching reaction finishes, filter, the sulfuric acid leached mud that obtains returns plumbous smelting system.Sulfuric acid leaches the main chemical reactions that takes place:
Cu(OH) 2+H 2SO 4＝CuSO 4+2H 2O (8)
CuCO 3+H 2SO 4＝CuSO 4+CO 2+H 2O (9)
Pb(OH) 2+H 2SO 4＝PbSO 4+2H 2O (10)
PbCO 3+H 2SO 4＝PbSO 4+CO 2+H 2O (11)
Na 2TeO 4+H 2SO 4＝Na 2SO 4+H 2TeO 4 (12)
The displacement of tellurium in 3 copper-baths
Sulfuric acid leaches the leach liquor obtain, is under 70～80 ℃ in temperature, adds weight and be the copper powder of 2.5～3.0 times of tellurium content in the leach liquor, reductase 12～5h.The main chemical reactions that reduction process takes place is:
H 2TeO 4+5Cu+6H +＝Cu 2Te↓+3Cu 2++4H 2O (13)
Described sodium hydroxide, yellow soda ash, sulfuric acid, copper powder, oxygen are technical grade reagent.
The present invention is suitable for the lead copper matte (lead matte) of Treatment of Copper lead ore concentrate melting output, and its composition scope is (%): Cu 10～50, and Pb 7.5～45, S8～29, Ni 0～10, and Se 0.2～4, and Te 0.1～3, and Au 0.07～3.5, Ag 0.02～0.20, and As 0.5～5, and Fe 0.5～15; Also be suitable for handling complicated copperized lead sulphide concentrate.
The treatment scheme of the present invention and existing lead copper matte relatively, following advantage is arranged: adopt alkaline pressure oxidation treatment lead copper matte, make the sulfide of copper, lead, tellurium etc. oxidized, be convenient to the Separation and Recovery of subsequent process, eliminated the sulfur dioxide flue gas of output in pyrogenic attack lead copper matte process and the pollution problem that leaded flue dust produces; When the alkaline oxygenated leached mud that pressurizes leaches with sulphuric acid soln, copper, tellurium and plumbous good separating effect, copper leaching yield reach more than 98%, the leaching yield of tellurium reaches more than 90%; Replace tellurium with copper powder in the copper-bath, the good and rate of recovery of tellurium removal effect is beneficial to focusing on of tellurium; Adopt the alkaline system pressure oxidation to leach, the material of equipment requires low, and alkaline medium is little to the corrosion of equipment, operational safety, and valuable metal comprehensively reclaims profitable; Labour intensity of the present invention is low, the treatment time short, good operational environment.
Description of drawings
Fig. 1: process flow diagram of the present invention.
Embodiment
Embodiment 1:
Lead ore concentrate is milled to granularity 100% less than 0.149mm through the lead copper matte of oxygen bottom blowing technology output, and its main component is (%): Cu 44.32 by weight percentage, and Pb 18.21, and S 16.50, and Se 0.74, and Te 0.21, and Ag 0.14, and As 0.61, and Fe 0.75; Industrial caustic soda, the wherein content of sodium hydroxide 〉=96%; Industrial sulphuric acid, wherein H 2SO 4Content 〉=98%; Industrial oxygen, wherein O 2Content 〉=99%; Industry copper powder, wherein copper content 〉=99%.
With the industrial caustic soda 85.0g of mentioned component, with 1200ml water wiring solution-forming and add the lead copper matte 200g of mentioned component, join after the pulp in the reactor that volume is 2000ml, airtight good reactor, the adjusting stirring velocity is 700～800r.min -1, feed industrial oxygen 5min and drive air remaining in the reactor.Then, when reactor was warming up to 160 ℃ gradually, feeding industrial oxygen and keeping oxygen partial pressure was 0.7MPa, and temperature of reaction rises to 218 ℃ fast behind 20min, descend subsequently, and temperature maintenance is reacted 1.5h at 200 ℃.After reaching the reaction times, in reactor, feed water coolant, when temperature is reduced to below 50 ℃, from reactor, emit slurry and filter filter residue 200ml water washing.The heavy 176.2g in leached mud oven dry back, it wants composition is (%): Cu 50.98 by weight percentage, and Pb 19.52, and S 0.9, and Se 0.015, and Te 0.22, and Ag 0.16, and As 0.49, and Fe 0.85, and the leaching yield of selenium is 98.20%; Leach liquor 1070ml, its composition (g/L) is: Na 2SO 4116.16 Pb 0.53, As 0.31, and Se 1.19, and NaOH 2.50.
With above-mentioned alkaline leached mud 176g, 1500ml sizes mixing with the 1.5mol/L sulphuric acid soln, and low whipping speed is 400r.min -1, temperature is 70 ℃ and leaches down 2h, leaches and finishes after-filtration, leached mud is dried after with the 150ml water washing, acid leached mud 62.48g, its major ingredient is (%): Cu 0.43 by weight percentage, and Pb 54.52, and S 8.37, Se 0.032, Te 0.053, and Ag 0.422, and As 0.96, Fe 1.01, and the leaching yield of copper and tellurium is respectively 99.7% and 90.65%; Obtain the copper-containing solution 1490ml that sulfuric acid leaches, its composition is (g/L): Cu 59.21, and Fe 0.55, and As 0.15, and Te 0.23.
With above-mentioned copper-bath 400ml, low whipping speed is 400r.min -1, temperature is under 85 ℃, adds copper powder 6g, reaction 2h reaches the reaction times after-filtration, obtain copper tellurium slag 0.93g, obtain except that the copper-bath 390ml behind the tellurium, its composition is (g/L): Cu 62.57, and Fe 0.53, As 0.14, and Te 0.001, and the cementation rate of tellurium is 99.57%.
Embodiment 2:
Lead ore concentrate is milled to granularity 100% less than 0.149mm through the lead copper matte of oxygen bottom blowing technology output, and its main component is (%): Cu 26.21 by weight percentage, and Pb 8.04, and S 10.50, and Se 0.40, and Ag 0.07, and As 0.82, and Fe 15.7; Industrial sodium carbonate, its content 〉=96%; Industrial sulphuric acid, wherein H 2SO 4Content 〉=98%; Industrial oxygen, wherein O 2Content 〉=99%.
With the industrial sodium carbonate 80.0g of mentioned component, the lead copper matte 200g with adding mentioned component behind the 1200ml water wiring solution-forming joins after the pulp in the pressure reaction still that volume is 2000ml.Airtight good reactor is opened and is stirred, and the adjusting stirring velocity is 700～800r.min -1, feed industrial oxygen 1min and drive air remaining in the reactor.Then, reactor is heated up gradually, when temperature rises to 160 ℃, feed industrial oxygen, keeping oxygen partial pressure is 0.7MPa, and temperature of reaction rises to 215 ℃ fast behind 20min, descend subsequently, and temperature maintenance is reacted 1.5h at 200 ℃.After reaching the reaction times, in reactor, feed water coolant, when temperature is reduced to below 50 ℃, from reactor, emit slurry and filter filter residue 200ml water washing.The heavy 164.7g in leached mud oven dry back, its main component is (%): Cu 32.51 by weight percentage, and Pb 9.18, and S 0.73, and Se 0.03, and Ag 0.09, and As 0.69, and Fe 18.91, and the leaching yield of selenium is 93.93%; Leach liquor 1030ml, its composition (g/L) is: Na 2SO 487.6 Pb 0.42, As 0.423, and Se 0.67, and pH 8.81.
With above-mentioned alkaline leached mud 150g, 900ml sizes mixing with the 1.5mol/L sulphuric acid soln, and low whipping speed is 400r.min -1, temperature is 70 ℃ and leaches down 2h, leach to finish after-filtration, leached mud is dried acid leached mud 61.2g after with the 100ml water washing, its major ingredient is (%): Cu 0.49 by weight percentage, Pb 22.37, and S 5.08, and Se 0.068, Ag 0.207, As 1.41, and Fe 23.17, and the leaching yield of copper is 99.39%; Obtain the copper-containing solution 892ml that sulfuric acid leaches, its composition is (g/L): Cu 52.73, and Fe 17.12, and As 0.17.

Claims (2)

1. the method for separating copper and selen-tellurjum from a lead copper matte is characterized in that being made up of following steps:
(1) oxidation is leached
Lead copper matte is earlier broken and wear into the powder that particle diameter is 0.25～0.074mm, with sodium hydroxide and sodium carbonate solution pulp and add in the autoclave, the back aerating oxygen that heats up carries out oxidizing reaction, the temperature of oxidizing reaction is 150～250 ℃, naoh concentration is 1.0～3.0mol/L, concentration of sodium carbonate is 0～2mol/L, the weight liquid-solid ratio that leaches is 3～10: 1, the dividing potential drop of oxygen is controlled at 0.3～1.5MPa, the total pressure of system maintains 1.5～3.5MPa, and the reaction times is 2～6h, after reaction finishes, be cooled to 20～60 ℃, filter;
(2) alkali soaks the sulfuric acid leaching of slag
The leached mud that obtains after the reaction is leached in oxidation, is under 70～85 ℃ in temperature, is that the sulphuric acid soln of 0.5～2.5mol/L is 2～8: 1 with the weight liquid-solid ratio with concentration, leach 2～3h, after sulfuric acid leaching reaction finishes, filter, the sulfuric acid leached mud that obtains returns plumbous smelting system;
(3) displacement of tellurium in the copper-bath
Sulfuric acid leaches the leach liquor obtain, is under 70～80 ℃ in temperature, adds weight and be the copper powder of 2.5～3.0 times of tellurium content in the leach liquor, reductase 12～5h.
2. according to claim 1 from lead copper matte the method for separating copper and selen-tellurjum, it is characterized in that: described sodium hydroxide, yellow soda ash, sulfuric acid, copper powder and oxygen are technical grade reagent.
CN2010102435118A 2010-08-03 2010-08-03 Method for separating copper, selenium and tellurium from lead matte Pending CN101935761A (en)

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Cited By (12)

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CN102586600A (en) * 2011-01-18 2012-07-18 郴州市金贵银业股份有限公司 Process for recycling valuable metal from lead copper matte
CN104947145A (en) * 2015-06-10 2015-09-30 云南驰宏锌锗股份有限公司 Method of balancing acid in high-lead copper sulphate oxygen pressure leaching-electrodepositing process
CN104975177A (en) * 2015-08-01 2015-10-14 西安西北有色地质研究院有限公司 Method for extracting copper from bound-type oxidized copper ore by wet process
CN105219958A (en) * 2015-11-16 2016-01-06 湖南城市学院 A kind of alkali oxide leaching is separated the method for selen-tellurjum enriching noble metals
CN105886785A (en) * 2015-01-25 2016-08-24 昆明冶金高等专科学校 Method for preparing high-purity silver powder from silver-rich residue containing high selenium and tellurium
CN106477533A (en) * 2016-10-19 2017-03-08 中南大学 A kind of method that copper anode mud separates and recovers selenium and tellurium
CN107190143A (en) * 2017-05-12 2017-09-22 江西铜业集团公司 The technique that a kind of Whote-wet method reclaims valuable element in complicated low-grade sulphide ore
CN107502748A (en) * 2017-09-11 2017-12-22 中南大学 A kind of method of Bellamya aeruginosa pressurization Strengthen education
CN108862212A (en) * 2018-08-31 2018-11-23 昆明鼎邦科技股份有限公司 A method of extracting tellurium from copper tellurium slag
CN109052339A (en) * 2018-08-31 2018-12-21 昆明鼎邦科技股份有限公司 A method of extracting tellurium from copper telluride or copper tellurium slag
CN111154977A (en) * 2020-02-06 2020-05-15 中国恩菲工程技术有限公司 Method for treating valuable metal sulfide concentrate
CN111172390A (en) * 2020-02-06 2020-05-19 中国恩菲工程技术有限公司 Method for treating valuable metal sulfide concentrate by oxygen pressure

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Cited By (16)

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Publication number Priority date Publication date Assignee Title
CN102586600A (en) * 2011-01-18 2012-07-18 郴州市金贵银业股份有限公司 Process for recycling valuable metal from lead copper matte
CN105886785A (en) * 2015-01-25 2016-08-24 昆明冶金高等专科学校 Method for preparing high-purity silver powder from silver-rich residue containing high selenium and tellurium
CN104947145A (en) * 2015-06-10 2015-09-30 云南驰宏锌锗股份有限公司 Method of balancing acid in high-lead copper sulphate oxygen pressure leaching-electrodepositing process
CN104975177A (en) * 2015-08-01 2015-10-14 西安西北有色地质研究院有限公司 Method for extracting copper from bound-type oxidized copper ore by wet process
CN104975177B (en) * 2015-08-01 2017-04-19 西安西北有色地质研究院有限公司 Method for extracting copper from bound-type oxidized copper ore by wet process
CN105219958B (en) * 2015-11-16 2018-08-24 湖南城市学院 A kind of method of alkali oxide leaching separation selen-tellurjum enriching noble metals
CN105219958A (en) * 2015-11-16 2016-01-06 湖南城市学院 A kind of alkali oxide leaching is separated the method for selen-tellurjum enriching noble metals
CN106477533A (en) * 2016-10-19 2017-03-08 中南大学 A kind of method that copper anode mud separates and recovers selenium and tellurium
CN107190143A (en) * 2017-05-12 2017-09-22 江西铜业集团公司 The technique that a kind of Whote-wet method reclaims valuable element in complicated low-grade sulphide ore
CN107502748A (en) * 2017-09-11 2017-12-22 中南大学 A kind of method of Bellamya aeruginosa pressurization Strengthen education
CN107502748B (en) * 2017-09-11 2018-09-25 中南大学 A kind of method of Bellamya aeruginosa pressurization enhanced leaching
CN108862212A (en) * 2018-08-31 2018-11-23 昆明鼎邦科技股份有限公司 A method of extracting tellurium from copper tellurium slag
CN109052339A (en) * 2018-08-31 2018-12-21 昆明鼎邦科技股份有限公司 A method of extracting tellurium from copper telluride or copper tellurium slag
CN111154977A (en) * 2020-02-06 2020-05-15 中国恩菲工程技术有限公司 Method for treating valuable metal sulfide concentrate
CN111172390A (en) * 2020-02-06 2020-05-19 中国恩菲工程技术有限公司 Method for treating valuable metal sulfide concentrate by oxygen pressure
CN111172390B (en) * 2020-02-06 2022-07-26 中国恩菲工程技术有限公司 Method for treating valuable metal sulfide concentrate by using oxygen pressure

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Application publication date: 20110105