CN1308466C - Production method of zinc indium by pressurized acid leaching neutralization precipitation separation indium from indium containing high iron zinc sulfide concentrate - Google Patents
Production method of zinc indium by pressurized acid leaching neutralization precipitation separation indium from indium containing high iron zinc sulfide concentrate Download PDFInfo
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- CN1308466C CN1308466C CNB2005100109448A CN200510010944A CN1308466C CN 1308466 C CN1308466 C CN 1308466C CN B2005100109448 A CNB2005100109448 A CN B2005100109448A CN 200510010944 A CN200510010944 A CN 200510010944A CN 1308466 C CN1308466 C CN 1308466C
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Abstract
The present invention belongs to a smelting method of indium-containing zinc sulphide concentrate. In the method, indium-containing zinc sulphide concentrate is milled and mixed with zinc electrodeposit liquid to form slurry entering a pressurizing reactor to be leached in acid to obtain zinc with the leaching rate of more than 99% and indium with the leaching rate of more than 92%; over 95% of indium in a leachate is separated by a neutralizing and precipitating method, so the indium has the recovery rate of more than 80% from the zinc concentrate to sponge indium. After the indium is separated from the leachate, metal zinc can be obtained through the steps of deironing, solution purification, electrodeposit, casting, etc. in the traditional wet zinc-smelting process. The method can simplify the process, bring high indium-zinc recovery rate and effectively process high-indium complicated zinc concentrate.
Description
Technical field
The invention belongs to the smelting process that contains the indium zinc sulfide concentrates, more particularly, relate to a kind of smelting process of from contain the indium high-iron zinc sulfide concentrate, extracting the zinc indium.
Background technology
Contain the indium high-iron zinc sulfide concentrate be meant iron content more than 10%, contain zinc be lower than 48% and association has higher scattered metals indium, the general name of the class zinc sulfide concentrates that iron can't be removed in ore dressing process.At present, for the processing that contains this class material of indium high-iron zinc sulfide concentrate, usually adopt traditional " fluidized bed roasting-calcining high temperature peracid leaches " technology, indium from iron vitriol slag or and slag in reclaim, the sulfur dioxide flue gas that high-iron zinc sulfide concentrate produces in roasting process reclaims through relieving haperacidity, but in sulfuric acid oversupply area, particularly there are not sour industrial area of consumption and traffic low developed area, the sulfuric acid that the sulfur dioxide flue gas that is produced by the roasting zinc sulfide concentrates reclaims, be subjected to having a strong impact on of sulfuric acid market, cause sulfuric acid to be difficult to effective utilization.Therefore, there is significant limitation in " roasting-leaching " smelting process.
In addition, there are defectives such as extraction of indium solution temperature height, solution-treated amount are big in the Technology of " the direct extracting and separating indium of pressurized acid leaching-leach liquor handle contain the indium high-iron zinc sulfide concentrate extract the metallic zinc indium " developed, this technology.
Summary of the invention
The present invention has overcome the deficiency of existing zinc ore concentrate smelting process, and what provide that a kind of smelting process do not produce that sulfur dioxide gas, extraction of indium liquor capacity greatly reduce contains indium high-iron zinc sulfide concentrate smelting process.
Realize that step of the present invention is: (1) contains the indium high-iron zinc sulfide concentrate and sulfur acid 140g/L～170g/L zinc electrodeposition waste liquid is sized mixing with fine ground, add in the autoclave then, 140 ℃～160 ℃ of controlled temperature, pressure 1.0MPa～1.6MPa, directly lead to the oxygen acidleach, valuable metals such as the zinc in the concentrate, indium, copper, cadmium are efficient simultaneously to be leached, and sulphur, lead, silver etc. are then stayed in the slag; (2) infusion solution of output is leached in pressurization, after 85 ℃～90 ℃ reduction is handled down, carries out the neutralization precipitation indium with zinc sulfide concentrates; (3) the precipitation of indium slag dissolves with sulphuric acid soln, with the organic extractant phase indium of P204 and kerosene composition, back extraction indium from load organic phases then, again with zinc metal sheet from the mid-sponge indium of getting in return of the back extraction indium aqueous solution; (4) leach liquor after the precipitate and separate indium adopts deironing in the Zinc hydrometallurgy process, solution purification, electrodeposition, founding operation, the output metallic zinc.Wherein: contain the indium high-iron zinc sulfide concentrate and contain indium 0.025%～0.09%, iron content 10%～25% contains zinc 38%～48%.Pressurized acid leaching is one section or two sections pressure leaching methods.
Beneficial effect of the present invention is: directly enter autoclave and lead to the oxygen acidleach because of containing indium high ferro zinc sulfide ore, the extraction temperature height, directly leach zinc, indium in the concentrate with the sulfuric acid in the zinc electrodeposition waste liquid, with the roasting in existing " roasting-leaching " technology, gather dust, leach and concentrate on pressurization and finish in the leaching process, make work simplification, process intensification is realized containing the efficient of indium zinc sulfide concentrates and is directly leached; Simultaneously, the sulphur in the concentrate is converted into elementary sulfur, after maturation process such as flotation, hot melt filtration are handled, obtain being convenient to the sulfur product that stores and transport, so main process is not subjected to the influence of sulfuric acid market and communications and transportation.Infusion solution separates indium through neutralization precipitation, the anti-molten and extraction of heavy indium slag, and the extraction solution treatment capacity significantly reduces, and has reduced production cost.
Description of drawings: accompanying drawing is a process flow sheet of the present invention.
Specific embodiment
Embodiment 1, contain the iron-holder 10% of indium high-iron zinc sulfide concentrate, contain indium 0.025%, zinc 38.0%, concentrate is levigate, and 98% crosses the 0.043mm sieve.
With levigate mistake contain the indium high-iron zinc sulfide concentrate and zinc electrodeposition waste liquid is sized mixing, in the acidproof autoclave that the adding volume is 4L, made by the titanium material, 140 ℃ of temperature, pressure 1.0MPa carry out one section continuously logical oxygen and leach.
The transformation efficiency 78.38% of zinc leaching rate 99.28%, indium leaching yield 94.43%, sulphur, leach liquor contains zinc 114.0g/L, contains indium 42.92mg/L.Leached mud contains zinc 0.67%, elementary sulfur 53.88%.
Leach liquor adds zinc sulfide concentrates reduction 90min under 85 ℃, add the limestone powder neutralization then, indium deposition rate 95.68%, obtain heavy indium slag In0.214%, heavy indium slag sulfuric acid dissolution, indium solubility rate 97.92%, solution contain In0.415g/L, Fe1.01g/L, with the organic phase 3 stage countercurrent extraction of indium that 20%P2O4 and 80% kerosene are formed, indium percentage extraction 98.49%; Load organic phases 3molHCl+2molZnCl
2Solution carries out the two-stage back extraction, and the indium back extraction ratio is 99.41%; From the back extraction indium aqueous solution, displace the sponge indium with zinc metal sheet.
Liquid adopts separation of iron in goethite form behind the heavy indium, and scum contains zinc 2.0%.After the deironing liquid purify respectively, electrodeposition, founding, obtain 1
#Zinc ingot metal.
Embodiment 2, contain the iron-holder 18% of indium high-iron zinc sulfide concentrate, contain indium 0.042%, zinc 40%, concentrate is levigate, and 99.0% crosses the 0.043mm sieve.
With levigate mistake contain the indium high-iron zinc sulfide concentrate and zinc electrodeposition waste liquid is sized mixing, add in the 4L titanium material autoclave, 150 ℃ of temperature, pressure 1.4MPa carry out one section continuously logical oxygen and leach.
The transformation efficiency 81.98% of zinc leaching rate 99.79%, indium leaching yield 98.02%, sulphur, leach liquor contains zinc 132g/L, contains indium 62.44mg/L.Leached mud contains zinc 0.87%, elementary sulfur 55.23%.
Leach liquor adds zinc sulfide concentrates reduction 90min under 90 ℃, add the limestone powder neutralization then, indium deposition rate 98.76%, obtain heavy indium slag In0.617%, heavy indium slag sulfuric acid dissolution, indium solubility rate 96.89%, solution contain In0.627g/L, Fe2.91g/L, with the organic phase 3 stage countercurrent extraction of indium that 20%P2O4 and 80% kerosene are formed, indium percentage extraction 98.91%; Load organic phases 3molHCl+2molZnCl
2Solution carries out the two-stage back extraction, and the indium back extraction ratio is 99.25%; From the back extraction indium aqueous solution, displace the sponge indium with zinc metal sheet.
Liquid adopts separation of iron in goethite form behind the heavy indium, and scum contains zinc 2.93%.After the deironing liquid purify respectively, electrodeposition, founding, obtain 1
#Zinc ingot metal.
Embodiment 3, contain the iron-holder 25% of indium high-iron zinc sulfide concentrate, contain indium 0.09%, zinc 48%, concentrate is levigate, and 98.5% crosses the 0.043mm sieve.
With levigate mistake contain the indium high-iron zinc sulfide concentrate and zinc electrodeposition waste liquid is sized mixing, in the acidproof autoclave that the adding volume is 4L, made by the titanium material, 160 ℃ of temperature, pressure 1.6MPa carry out two sections continuously logical oxygen and leach.
The transformation efficiency 79.62% of zinc leaching rate 99.48%, indium leaching yield 98.21%, sulphur, leach liquor contains zinc 141g/L, contains indium 55.63mg/L.Leached mud contains zinc 1.02%, elementary sulfur 52.42%.
Leach liquor adds zinc sulfide concentrates reduction 90min under 95 ℃, add the limestone powder neutralization then, indium deposition rate 97.91%, obtain heavy indium slag In0.511%, heavy indium slag sulfuric acid dissolution, indium solubility rate 97.23%, solution contain In0.564g/L, Fe3.49g/L, with the organic phase 3 stage countercurrent extraction of indium that 20%P2O4 and 80% kerosene are formed, indium percentage extraction 98.23%; Load organic phases 3molHCl+2molZnCl
2Solution carries out the two-stage back extraction, and the indium back extraction ratio is 99.45%; From the back extraction indium aqueous solution, displace the sponge indium with zinc metal sheet.
Liquid adopts separation of iron in goethite form behind the heavy indium, and scum contains zinc 3.01%.After the deironing liquid purify respectively, electrodeposition, founding, obtain 1
#Zinc ingot metal.
Claims (6)
1, a kind of indium high-iron zinc sulfide concentrate pressurized acid leaching-neutralization precipitation that contains separates indium production zinc indium method, the steps include:
(1) contain the indium high-iron zinc sulfide concentrate and sulfur acid 140g/L～170g/L zinc electrodeposition waste liquid is sized mixing with fine ground, add then in the autoclave, 140 ℃～160 ℃ of controlled temperature, pressure 1.0MPa～1.6MPa directly leads to the oxygen acidleach;
(2) infusion solution of output is leached in pressurization, after 85 ℃～95 ℃ reduction of temperature are handled, carries out the neutralization precipitation indium with zinc sulfide concentrates;
(3) the precipitation of indium slag dissolves with sulphuric acid soln, with the organic extractant phase indium of P204 and kerosene composition, back extraction indium from load organic phases then, again with zinc metal sheet from the mid-sponge indium of getting in return of the back extraction indium aqueous solution;
(4) leach liquor after the precipitate and separate indium adopts deironing in the Zinc hydrometallurgy process, solution purification, electrodeposition, founding operation, the output metallic zinc.
2, the indium high-iron zinc sulfide concentrate pressurized acid leaching-neutralization precipitation that contains according to claim 1 separates indium production zinc indium method, and it is characterized in that: the described indium high-iron zinc sulfide concentrate that contains contains indium 0.025%～0.09%.
3, the indium high-iron zinc sulfide concentrate pressurized acid leaching-neutralization precipitation that contains according to claim 1 separates indium production zinc indium method, it is characterized in that: the described indium high-iron zinc sulfide concentrate iron content 10%～25% that contains.
4, the indium high-iron zinc sulfide concentrate pressurized acid leaching-neutralization precipitation that contains according to claim 1 separates indium production zinc indium method, and it is characterized in that: the described indium high-iron zinc sulfide concentrate that contains contains zinc 38%～48%.
5, the indium high-iron zinc sulfide concentrate pressurized acid leaching-neutralization precipitation that contains according to claim 1 separates indium production zinc indium method, and it is characterized in that: described pressurized acid leaching is one section pressure leaching method.
6, the indium high-iron zinc sulfide concentrate pressurized acid leaching-neutralization precipitation that contains according to claim 1 separates indium production zinc indium method, and it is characterized in that: described pressurized acid leaching is two sections pressure leaching methods.
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| CNB2005100109448A CN1308466C (en) | 2005-07-28 | 2005-07-28 | Production method of zinc indium by pressurized acid leaching neutralization precipitation separation indium from indium containing high iron zinc sulfide concentrate |
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| CN1308466C true CN1308466C (en) | 2007-04-04 |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100393896C (en) * | 2007-01-22 | 2008-06-11 | 中国科学院过程工程研究所 | New method for soaking out enriched ores of high indium, high iron, and high sulfur zinc |
| CN101717868B (en) * | 2009-12-01 | 2011-03-30 | 南京中锗科技股份有限公司 | Method for comprehensively recovering indium and gallium from distilled waste acid containing indium and gallium |
| CN101798639B (en) * | 2009-12-16 | 2011-06-08 | 株洲冶炼集团股份有限公司 | Method for recovering indium from indium-containing neutralized dregs directly leached from zinc concentrate |
| CN102134654A (en) * | 2010-01-21 | 2011-07-27 | 云南冶金集团股份有限公司 | Treatment method of zinc sulfide ore concentrates |
| CN102051489A (en) * | 2011-01-14 | 2011-05-11 | 上海大学 | Method for recycling indium from acid pressure oxidative leaching liquid of zinc smelting product |
| CN102747233B (en) * | 2012-07-18 | 2014-01-22 | 昆明冶金研究院 | Sulfur concentrate recovery process in pre-cavitation and sulfur flotation of zinc oxidative pressure leaching residue |
| CN102766765B (en) * | 2012-08-07 | 2014-12-24 | 四川四环电锌有限公司 | Zinc oxide powder recycling method |
| CN102787241B (en) * | 2012-09-10 | 2013-08-21 | 云南东昌金属加工有限公司 | Method for extracting and recycling indium from chlorination distillation residue liquid generated after germanium extraction of germanium ore concentrate |
| CN103194599A (en) * | 2013-04-25 | 2013-07-10 | 大兴安岭云冶矿业开发有限公司 | Method for processing zinc sulfide concentrated ore |
| 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 |
| CN104451206A (en) * | 2014-12-13 | 2015-03-25 | 株洲冶炼集团股份有限公司 | Process for increasing reclamation rate of indium in zinc concentrate |
| CN105886797A (en) * | 2015-01-25 | 2016-08-24 | 昆明冶金高等专科学校 | Method for preparing sponge indium from polymetallic sulfide material |
| CN105002354A (en) * | 2015-07-28 | 2015-10-28 | 昆明理工大学 | Method for leaching zinc and other valuable metal in zinc sulfide ore through medium-and-low-pressure oxygen enrichment |
| CN105695752A (en) * | 2016-03-29 | 2016-06-22 | 云南华联锌铟股份有限公司 | Method for recycling indium from indium containing material produced during zinc smelting |
| CN106893873B (en) * | 2016-12-28 | 2018-11-27 | 呼伦贝尔驰宏矿业有限公司 | A kind of zinc sulphide containing indium, silver, arsenic is total to association concentrate zinc metallurgy method |
| CN113373323B (en) * | 2021-04-28 | 2022-12-06 | 中南大学 | Method for recovering indium from high-iron indium-containing waste liquid |
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