CN102618719A - Method for directly leaching zinc and recovering gallium, germanium and indium from zinc sulfide concentrate - Google Patents

Method for directly leaching zinc and recovering gallium, germanium and indium from zinc sulfide concentrate Download PDF

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Publication number
CN102618719A
CN102618719A CN2012101123993A CN201210112399A CN102618719A CN 102618719 A CN102618719 A CN 102618719A CN 2012101123993 A CN2012101123993 A CN 2012101123993A CN 201210112399 A CN201210112399 A CN 201210112399A CN 102618719 A CN102618719 A CN 102618719A
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China
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zinc
send
pressure
indium
germanium
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CN2012101123993A
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Chinese (zh)
Inventor
何醒民
潘晨湘
余刚
李夏湘
左小红
邓孟俐
蔡江松
徐毅
刘野平
张登凯
林裕安
王李娟
Original Assignee
长沙有色冶金设计研究院有限公司
深圳市中金岭南有色金属股份有限公司丹霞冶炼厂
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Priority to CN2012101123993A priority Critical patent/CN102618719A/en
Publication of CN102618719A publication Critical patent/CN102618719A/en

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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a method for directly leaching zinc and recovering gallium, germanium and indium from zinc sulfide concentrate. The method comprises the following steps of: grinding the zinc sulfide concentrate, directly leaching the zinc sulfide concentrate at a low temperature under a low pressure by adopting low acid, leaching the leached slag at a high temperature under a high pressure by adopting high acid, neutralizing and displacing the leachate, conveying the filter residue to a gallium, germanium and indium recovery system, removing iron from the filtrate, purifying, performing electro-deposition, and smelting to produce zinc ingots. By the method, the zinc can be directly leached from the zinc sulfide concentrate, and dissipated metals such as gallium, germanium and indium are comprehensively recovered when the zinc is recovered.

Description

Directly leach the method for zinc and recovery gallium germanium indium from zinc sulfide concentrates

Technical field

The invention belongs to technical field of wet metallurgy, be specifically related to a kind of method that directly leaches zinc and recovery gallium germanium indium from zinc sulfide concentrates.

Background technology

From zinc leaching residue, reclaim at present the technology of gallium, germanium, indium, research and application are at home and abroad all arranged, conclude and get up to mainly contain following several method.

1, chloride volatility process

Chloride volatility process is in zinc leaching residue, to add the chlorizating agent roasting; Gallium, germanium, indium are separated out recovery, reduction-sulfurization melting and direct magnetic separation preconcentration and separation technology with the volatilization of chloride form high-temp chlorination; The greatest problem that this method exists is a muriate to corrosion on Equipment and to the pollution of environment, and technical indicator is also undesirable.

2, Porto-Marghera method

This method is that carbon dust is allocated in the zinc leaching residue; Adopt rotary kiln at high temperature to reduce fuming; Make most of gallium, germanium, indium get into flue dust, then flue dust is carried out alkali cleaning defluorinate chlorine, molten deposition, extraction process recovery gallium, germanium, the indium of reaching of reductinic acid, this method is because the employing high-temperature roasting; Exist and to gather dust and atmosphere polluting problem, and low at rotary kiln reduction volatilization operation gallium, germanium, indium recovery.

3, rhombohedral iron ore-extraction process

Zinc leaching residue is at first through high pressure SO 2Reduction is leached, and makes most of gallium, germanium, indium get into leach liquor, and leach liquor reclaims gallium, germanium, indium through multi-stage solvent extraction again after the heavy gallium that neutralizes, germanium, indium are the enrichment slag, and neutralization back liquid is through the hematite process deironing, and this method technical process is long and complicated, and production cost is higher.

Above several method is from zinc leaching residue, to reclaim gallium, germanium, indium, and research and application result show, when reclaiming main metallic zinc, comprehensively reclaim dissipated metal gallium, germanium, indium, adopts wet method than adopting the pyrogenic process better effects if.Dissipated metal and iron close relation, iron leaches, and gallium, germanium, indium are also leached thereupon; In conventional zinc hydrometallurgy roasting process, because forming low acid with iron, the part zinc of zinc ore concentrate is difficult to the dissolved zinc ferrite, gallium, germanium, indium are with in the class matter homophase entering zinc ferrite lattice and lose; Be full wet processing and directly leach; Not needing the zinc ore concentrate roasting process, do not produce zinc ferrite, is the most suitable technology that directly from zinc ore concentrate rather than zinc leaching residue, comprehensively reclaims dissipated metal.

Directly leaching is that a kind of the smelting for efficient and environmental protection wet method zinc researched and developed, and generally is divided into several kinds of modes:

1, one section low acid is directly leached: 145~155 ℃ of temperature, pressure 1100~1300kPa, acidity 20~30g/l.

2, one section peracid directly leaches: 145~155 ℃ of temperature, pressure 1100~1300kPa, acidity 50~60g/l.

3, two sections adverse currents directly leach: 145~155 ℃ of temperature, pressure 1100~1300kPa, acidity 30~40g/l.

4, two sections and directly leaching of stream: 145~155 ℃ of temperature, pressure 1100~1300kPa, acidity 60~80g/l.

Adopt the HTHP direct leaching process, the supernatant iron content major part of generation is Fe 3+, the iron of leaching and gallium, germanium, indium difficulty separate, and can only reclaim main metallic zinc.In addition, HTHP directly leaches zinc sulfide concentrates, and most of iron is left in the leached mud, and it is big to leach the quantity of slag.

Summary of the invention

The purpose of this invention is to provide and a kind ofly directly leach zinc and reclaim the method for gallium germanium indium from zinc sulfide concentrates, this method can directly leach zinc and the comprehensive dissipated metal gallium germanium indium that reclaims when reclaiming zinc from zinc sulfide concentrates.

This method that directly leaches zinc and reclaim gallium germanium indium from zinc sulfide concentrates provided by the invention comprises the following steps:

(1) pumps into first stage reactor after grinding zinc sulfide concentrates well, feed the oxygen of concentration more than 98%, directly leaching of the low acid of low-temp low-pressure in first stage reactor; The low sour controlled temperature of said low-temp low-pressure is 105~120 ℃; Pressure is 200~350kPa, and acidity is 10~20g/l, leaches ore pulp after the flash drum decrease temperature and pressure; Send one section thickener to separate, obtain leach liquor and leached mud;

(2) the said leached mud of step (1) is pumped into second stage reactor, feed the oxygen of concentration more than 98%, add waste electrolyte simultaneously; The HTHP peracid leaches, and said HTHP peracid controlled temperature is 145~155 ℃, and pressure is 1100~1300kPa; Acidity is 60~80g/l, leaches ore pulp after the flash drum decrease temperature and pressure, send two sections thickeners to separate; Supernatant send first stage reactor, and underflow send the floatation recovery elementary sulfur, and mine tailing is rich lead skim;

(3) the said leach liquor of step (1) is sent into neutralizing well, add calcining and make neutralizing agent, controlled temperature is 70-80 ℃, and neutralization back ore pulp send the pressure filter filtering separation, and filter residue send first stage reactor, and filtrating is sent displacement slot;

(4) add zinc powder in the filtrating in displacement slot, controlled temperature 70-80 ℃, the terminal point pH value is 5-5.2, and reacted filter residue send gallium, germanium, indium recovery system, and displacement filtrating is sent iron removal trough;

(5) in iron removal trough, add calcining, blast pressurized air, 80~90 ℃ of controlled temperature, iron removal pH value is controlled at 3.0~4.0, and ore pulp send thickener to separate after the deironing, and filter residue is that scum send Rotary Kiln to handle, and filtrating is sent purification, electrodeposition, founding output zinc ingot metal.

The present invention compares with traditional method, has the following advantages:

1, the present invention adopts low-temp low-pressure to hang down sour processing condition, 105~120 ℃ of temperature, and pressure 200~350kPa has solved the iron that leaches and gallium, germanium, indium separation problem.

2, the present invention directly leaches from zinc sulfide concentrates, and the supernatant iron content major part of generation is Fe 2+, for favourable condition has been created in the recovery of dissipated metal.

3, the present invention directly leaches zinc sulfide concentrates, utilizes zinc ore concentrate directly in reactor drum, to reduce Fe 3+Become Fe 2+, leaching and reduction are accomplished in same reactor drum, do not need independent reactor drum to make reduction process.

4, the present invention directly leaches zinc sulfide concentrates, and most of iron is leached to be got in the supernatant, and it is few to leach the quantity of slag.

5, the supernatant iron content of output of the present invention is Fe 2+, adopt the method for the heavy gallium of neutralization displacement, germanium, indium, iron is separated with gallium, germanium, indium, gallium, germanium, indium are precipitated as enriched substance and make raw material and further reclaim gallium, germanium, indium.

6, the supernatant of output of the present invention is behind the heavy gallium of neutralization displacement, germanium, indium, and iron is stayed and is Fe in the supernatant 2+, adopt atmospheric oxidation Fe 2+Be Fe 3+After, in and deironing, iron is with pyrrhosiderite pattern precipitate and separate.

Description of drawings

Fig. 1 is a process flow sheet of the present invention.

Embodiment

Technical process as can beappreciated from fig. 1 of the present invention, its practical implementation step is:

(1) zinc ore concentrate will pump into first stage reactor through about granularity behind the ore grinding about 25~40 μ m, feed the oxygen of concentration more than 98%; Adopt the low acidleach of low-temp low-pressure to go out; Temperature is in 105~120 ℃ of scopes, and pressure is in 200~350kPa scope, and acidity is in 10~20g/l scope.The temperature that this embodiment adopts is 110 ℃, and pressure is 300kPa, and acidity is 15g/l.Make so that sulphur is oxidized to elementary sulfur in the zinc sulphide, zinc becomes solvable zinc sulfate, leaches ore pulp after the flash drum decrease temperature and pressure, send one section thickener to separate, and one section supernatant promptly leaches solution of zinc sulfate.

(2) one section thickener underflow is pumped into second stage reactor, feed the oxygen of concentration more than 98%, add waste electrolyte simultaneously; Adopt the HTHP peracid to leach 145~155 ℃ of temperature, pressure 1100~1300kPa; Acidity is in 60~80g/l scope; The temperature that this embodiment adopts is 150 ℃, and pressure is 1200kPa, and acidity is 70g/l.Leach ore pulp after the flash drum decrease temperature and pressure, send two sections thickeners to separate, supernatant send first stage reactor, and underflow send the floatation recovery elementary sulfur, and mine tailing is that rich lead skim can be sold outward.

(3) one sections supernatants get into neutralizing well, and add calcining and make neutralizing agent, 70~80 ℃ of controlled temperature, neutralization back ore pulp send the pressure filter filtering separation, and filter residue send first stage reactor; Filtrating is sent displacement slot, adds zinc powder, 70~80 ℃ of controlled temperature, endpoint pH 5~5.2; Filter residue send gallium, germanium, indium recovery system, and displacement filtrating is sent iron removal trough, adds calcining, blasts pressurized air; 80~90 ℃ of controlled temperature, iron removal pH value is controlled at 3.0~4.0, and ore pulp send thickener to separate after the deironing, and filter residue is that scum send Rotary Kiln to handle; Obtain scum and zinc oxide fumes, filtrating is sent purification, electrodeposition, and waste electrolyte is sent into second stage reactor behind the electrodeposition, zinc metal sheet founding output zinc ingot metal.

Claims (2)

1. one kind is directly leached zinc and reclaims the method for gallium germanium indium from zinc sulfide concentrates, and this method comprises the following steps:
(1) pumps into first stage reactor after grinding zinc sulfide concentrates well, feed the oxygen of concentration more than 98%, directly leaching of the low acid of low-temp low-pressure in first stage reactor; The low sour controlled temperature of said low-temp low-pressure is 105~120 ℃; Pressure is 200~350kPa, and acidity is 10~20g/l, leaches ore pulp after the flash drum decrease temperature and pressure; Send one section thickener to separate, obtain leach liquor and leached mud;
(2) the said leached mud of step (1) is pumped into second stage reactor, feed the oxygen of concentration more than 98%, add waste electrolyte simultaneously; The HTHP peracid leaches, and said HTHP peracid controlled temperature is 145~155 ℃, and pressure is 1100~1300kPa; Acidity is 60~80g/l, leaches ore pulp after the flash drum decrease temperature and pressure, send two sections thickeners to separate; Supernatant send first stage reactor, and underflow send the floatation recovery elementary sulfur, and mine tailing is rich lead skim;
(3) the said leach liquor of step (1) is sent into neutralizing well, add calcining and make neutralizing agent, controlled temperature is 70-80 ℃, and neutralization back ore pulp send the pressure filter filtering separation, and filter residue send first stage reactor, and filtrating is sent displacement slot;
(4) add zinc powder in the filtrating in displacement slot, controlled temperature 70-80 ℃, the terminal point pH value is 5-5.2, and reacted filter residue send gallium, germanium, indium recovery system, and displacement filtrating is sent iron removal trough;
(5) in iron removal trough, add calcining, blast pressurized air, 80~90 ℃ of controlled temperature, iron removal pH value is controlled at 3.0~4.0, and ore pulp send thickener to separate after the deironing, and filter residue is that scum send Rotary Kiln to handle, and filtrating is sent purification, electrodeposition, founding output zinc ingot metal.
2. according to claim 1ly directly leach zinc and reclaim the method for gallium germanium indium, it is characterized in that its granularity of the good back of the mill of zinc sulfide concentrates described in the step (1) is 25~40 μ m from zinc sulfide concentrates.
CN2012101123993A 2012-04-17 2012-04-17 Method for directly leaching zinc and recovering gallium, germanium and indium from zinc sulfide concentrate CN102618719A (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102796868A (en) * 2012-09-12 2012-11-28 长沙有色冶金设计研究院有限公司 Production process for directly leaching zinc from zinc sulfide concentrate
CN103160688A (en) * 2013-04-17 2013-06-19 昆明奥赛美科技有限公司 Method for preparing germanium concentrate from germanium-containing leachate through utilizing zinc powder replacement method
CN103290214A (en) * 2013-05-28 2013-09-11 中国恩菲工程技术有限公司 Method for depositing iron from ferruginous zinc sulfate solution
CN103305692A (en) * 2013-05-28 2013-09-18 中国恩菲工程技术有限公司 Leaching method of zinc sulfide concentrate
CN103866120A (en) * 2014-03-25 2014-06-18 长沙有色冶金设计研究院有限公司 Method for leaching zinc and recovering valuable metals through carrying out pressurized oxidation on zinc sulfide concentrates
CN103882228A (en) * 2013-12-20 2014-06-25 河南豫光锌业有限公司 Method for enrichment and recovery of gallium and germanium from raffinate of indium smelting system
CN104120252A (en) * 2014-07-25 2014-10-29 长沙有色冶金设计研究院有限公司 Ore pulp cooling method and device for pressurized oxygen leaching of zinc sulfide concentrate
CN105063372A (en) * 2015-07-30 2015-11-18 云南驰宏锌锗股份有限公司 Method for purifying germanium in zinc sulfate solution through magnetic seeds
CN107287422A (en) * 2017-08-16 2017-10-24 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 Continuous deferrization technique in zinc hydrometallurgy
CN108130431A (en) * 2017-12-04 2018-06-08 云南驰宏资源综合利用有限公司 A kind of richness germanium zinc concentrate oxygen leaching inhibits the method that germanium leaches
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
CN108987841A (en) * 2018-08-28 2018-12-11 湖南邦普循环科技有限公司 A method of recycling valuable metal from waste and old lithium ion battery
CN109055749A (en) * 2018-09-28 2018-12-21 长沙有色冶金设计研究院有限公司 A kind of processing method of zinc oxygen leaching solution

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102796868A (en) * 2012-09-12 2012-11-28 长沙有色冶金设计研究院有限公司 Production process for directly leaching zinc from zinc sulfide concentrate
CN103160688A (en) * 2013-04-17 2013-06-19 昆明奥赛美科技有限公司 Method for preparing germanium concentrate from germanium-containing leachate through utilizing zinc powder replacement method
CN103160688B (en) * 2013-04-17 2015-08-05 昆明奥赛美科技有限公司 Zinc replacement prepares the method for germanium concentrate from germanic leach liquor
CN103290214A (en) * 2013-05-28 2013-09-11 中国恩菲工程技术有限公司 Method for depositing iron from ferruginous zinc sulfate solution
CN103305692A (en) * 2013-05-28 2013-09-18 中国恩菲工程技术有限公司 Leaching method of zinc sulfide concentrate
CN103305692B (en) * 2013-05-28 2016-06-01 中国恩菲工程技术有限公司 Zinc sulfide concentrates leaching method
CN103882228A (en) * 2013-12-20 2014-06-25 河南豫光锌业有限公司 Method for enrichment and recovery of gallium and germanium from raffinate of indium smelting system
CN103866120A (en) * 2014-03-25 2014-06-18 长沙有色冶金设计研究院有限公司 Method for leaching zinc and recovering valuable metals through carrying out pressurized oxidation on zinc sulfide concentrates
CN103866120B (en) * 2014-03-25 2016-03-16 长沙有色冶金设计研究院有限公司 Zinc sulfide concentrates pressurised oxygen Leaching Zinc reclaims the method for valuable metal simultaneously
CN104120252A (en) * 2014-07-25 2014-10-29 长沙有色冶金设计研究院有限公司 Ore pulp cooling method and device for pressurized oxygen leaching of zinc sulfide concentrate
CN105063372A (en) * 2015-07-30 2015-11-18 云南驰宏锌锗股份有限公司 Method for purifying germanium in zinc sulfate solution through magnetic seeds
CN107287422A (en) * 2017-08-16 2017-10-24 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 Continuous deferrization technique in zinc hydrometallurgy
CN107287422B (en) * 2017-08-16 2019-09-24 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 Continuous deferrization technique in zinc hydrometallurgy
CN108130431A (en) * 2017-12-04 2018-06-08 云南驰宏资源综合利用有限公司 A kind of richness germanium zinc concentrate oxygen leaching inhibits the method that germanium leaches
CN108130431B (en) * 2017-12-04 2019-09-20 云南驰宏资源综合利用有限公司 A kind of method that richness germanium zinc concentrate oxygen leaching inhibits germanium to leach
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
CN108987841A (en) * 2018-08-28 2018-12-11 湖南邦普循环科技有限公司 A method of recycling valuable metal from waste and old lithium ion battery
CN109055749A (en) * 2018-09-28 2018-12-21 长沙有色冶金设计研究院有限公司 A kind of processing method of zinc oxygen leaching solution

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Application publication date: 20120801