CN102560157A - Method for reclaiming zinc and indium from high-iron low-zinc multi-metal tailings - Google Patents
Method for reclaiming zinc and indium from high-iron low-zinc multi-metal tailings Download PDFInfo
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- CN102560157A CN102560157A CN2012100405225A CN201210040522A CN102560157A CN 102560157 A CN102560157 A CN 102560157A CN 2012100405225 A CN2012100405225 A CN 2012100405225A CN 201210040522 A CN201210040522 A CN 201210040522A CN 102560157 A CN102560157 A CN 102560157A
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- stibium
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Abstract
The invention provides a method for reclaiming zinc and indium from high-iron low-zinc multi-metal tailings, and discloses an environment-friendly method for treating aluminum slag generated in tin smelting process. The method comprises the following steps of: reducing and smelting aluminum slag through a vertical furnace, wherein harmful elements including arsenic and stibium in the aluminum slag react with tin to generate tin-arsenic-stibium alloy; and electrolyzing the tin-arsenic-stibium alloy to generate soldering tin and tin-arsenic-silver enriched anode sludge so as to achieve the aim of separating tin from arsenic and stibium. The aluminum slag generated when arsenic and stibium are removed by adding aluminum in tin smelting is treated by the vertical furnace, wherein the aluminum slag and slagging material auxiliaries are filled in a crucible and put in the vertical furnace, then subjected to thermal reduction to obtain the tin-arsenic-stibium alloy and poor-tin slag, the tin-stibium alloy is electrolyzed to obtain soldering tin and tin-arsenic-silver enriched anode sludge, and antimony white and noble metals can be additionally reclaimed from the anode sludge. The method has the advantages that: firstly, the coal consumption is low, 0.8-1.0t of coal is consumed for treating 1t of aluminum slag; secondly, the tin reclamation rate is high, which reaches 95 to 99 percent, the aluminum can be separated when entering the poor-tin slag; and thirdly, the method has small equipment investment, low production cost, small vertical furnace investment and lower coal consumption, and 0.8-1.0t of coal consumption for treating 1t of aluminum slag achieves the aims of economy and environmental friendliness.
Description
Technical field
The invention belongs to and utilize hydrometallurgy, be specifically related to a kind of method of from the low zinc multi-metal tailings of high ferro, extracting indium.
Background technology
Because the exhaustion of zinc ore concentrate resource, the comprehensive recovery new technology of preparing of the low zinc multi-metal tailings of the high ferro in mining, the ore dressing has become the important component part of the novel industry of China's strategy.At present, in various pyrogenic processes and wet method smelting process, the low zinc multi-metal tailings of high ferro does not have the process introduction of individual curing; Generally join miningly as zinc ore concentrate, consumption is few, and ubiquity zinc, indium recovery are low; Technical process is long, and production cost is high, and silver-colored tin is difficult to problems such as recovery.Publication number is that CN1272553 discloses new process for recovering metals such as a kind of indium of handling high indium high-iron zinc sulfide concentrate, iron, silver, tin on Chinese patent.
This technology is to carry out iron content greater than 10% zinc ore concentrate adopting hot acid to leach earlier through oxidizing roasting, makes zinc, indium, iron 95% or more get into solution, in tin, the silver entering slag; With the heavy iron of jarosite process, the indium of solution 98%, iron get in the iron vitriol slag, accomplish separating of zinc and indium, iron again for zinc, indium, ferrous solution; Iron vitriol slag is used the rotary kiln reduction volatilization, obtains the scum of rich indium secondary zinc oxide and about 30%.The secondary zinc oxide acidleach, indium is carried in extraction then, and scum is as cement, brick-making raw material.Tin silver slag reduces with charcoal, obtains the stanniferous silver preparation concentrate and takes out.This technical process is long, and the recovery of indium is low, has only 70%, and the slag rate of going into of silver has only 95%, and the slag rate of going into of tin has only 80%.
Summary of the invention
The object of the present invention is to provide a kind of technical process short, the recovery is high, and cost is low, the method for from the low zinc multi-metal tailings of high ferro, extracting indium that silver-colored enrichment is of high grade.
Method of the present invention may further comprise the steps:
1, disk pelletizing: after volume ratio is mixed at 3: 1 by weight with the vitriol oil with the low zinc multi-metal tailings of water content 6～8% high ferros, on the disk pelletizing machine, process the particle of 3-5mm size, tail gas entering exhaust treatment system, its reaction formula is following:
Me+2H
2SO
4＝Me?SO
4+SO
2+2↑H
2O
MeS+2H
2SO
4＝Me?SO
4+SO
2+2↑H
2O+S
0
MeS+4H
2SO
4＝Me?SO
4+4SO
2+4↑H
2O
Zn
2SiO
4+2H
2SO
4＝2Zn?SO
4+SiO
2+7H
2O
MeO+H
2SO
4＝Me?SO
4+H
2O
2, acidizing fired: as will to process the particulate material and evenly put into and carry out roasting in the rotary kiln; Temperature is controlled at 400 ℃～650 ℃, and 2～3 hours time, flue gas gathers dust through surface cool device and pulsating collection device; Emptying after the ammonia process tail gas unit is handled again; Calcining release grinding system is put into calcine bin, and the collected ash of surface cool device and pulsating collection device reclaims other rare metals;
3, the hot acid of calcining leaches and the reduction of iron: the calcining that will pass through behind the ball milling adds initial acid 180～200
In the g/L sulphuric acid soln, liquid-solid ratio 5-6: 1,85～90 ℃ of temperature are incubated 5～6 hours, in temperature-rise period, add the pyrolusite of 8～10% calcining weight; Before the press filtration, analyze Fe
3+, calculate the iron powder amount (iron content is greater than 88%) that adds, sampling filtering, filtrating is used the Rhocya titration again, nondiscoloration, press filtration obtains being rich in silver-colored scruff and contains indium, zinc, ferrous solution.Contain indium, zinc, ferrous solution and send the indium extraction, rich silver-colored scruff is managed elsewhere, and its reaction formula is following:
ZnO+H
2SO
4＝Zn?SO
4+H
2O
In+3H
2SO
4＝In
2(SO
4)
3+3H
2↑
In
2O
3+3H
2SO
4＝In
2(SO
4)
3+3?H
2O
2InAsO
4+3H
2SO
4＝In
2(SO
4)
3+2H
3?AsO
4
Fe
2O
3+3H
2SO
4＝Fe
2(SO
4)
3+3H
2O
ZnO.Fe
2O
3+4H
2SO
4＝Fe
2(SO
4)
3+4?H
2O+Zn?SO
4
Fe
3++Fe＝2Fe
2+
4, the extraction of indium: 25% P is adopted in extraction
20
4, thinner is a kerosene, extracts 8 grades; Water: organic phase=6: 1, temperature 10-45 ℃, raffinate returns the electrolytic zinc system; The reverse-extraction agent that back extraction is adopted is a hydrochloric acid, 3 grades of back extractions; Water: organic phase=1: 15;
5, the solution of indium of back extraction is sent into displacement slot, replace, make indium be reduced to zeroth order, get the sponge indium with zinc metal sheet;
6, the founding of indium: producing the sponge indium by the displacement operation and press group, send casting furnace to carry out founding, carry out electrolysis again, must purity be 99.99% electrolysis indium.
Raffinate returns the electrowinning zinc system, utilizes the patent No. ZL200810143744.3 of our company patent of invention raffinate to neutralize with secondary zinc oxide, and precipitating alum and removing iron purifies, electrodeposition, and founding obtains zinc ingot metal No. one
The present invention adds the vitriol oil with high ferro high ferro zinc-silver indium tin-polymetallic mine tailing to carry out roasting together; After calcining and the flue dust that obtains vitriol is ground to the 80-100 order together; Carry out the high temperature peracid again and leach the also direct iron powder reducing of using; The solution of press filtration send indium workshop section to reclaim indium and zinc, and the Gao Xiyin slag reclaims tin and silver in addition.This method technical process is short, and the recovery is high, and cost is low, and the enrichment of silver is of high grade, and the recovery of Zn reaches more than 99%.The recovery of In reaches more than 95%.In 99% the Ag enrichment slag, in 90% the tin enrichment slag; Solved mine tailing unmanageable problem in hydrometallurgy of high ferro, high silicon; Silver, the rich rate height of tin, preparation silver and tin product easily.
Description of drawings:
Fig. 1 is a concrete process flow sheet of the present invention.
Embodiment according to the technical process of Fig. 1 is implemented is following:
Embodiment one
Raw material: multi-metal tailings 500 grams.Composition:
| Element term | Zn％ | In(g/t) | Ag(g/t) | Fe％ | Sn％ | H 2O％ | S％ |
| Percentage composition | 22.79 | 1431 | 348 | 22 | 5 | 8 | 19 |
Manganese powder MO
2Greater than 55%
Sulfuric acid H
2SO
4Greater than 93%
Iron powder Fe is greater than 88%
Acidizing fired: the multi-metal tailings of getting 500g adds the 166ml vitriol oil and stirs in Stainless steel basin, puts into 650 ℃ retort furnace roasting 2.5-3 hour then, and take out the cooling back, clays into power.
Leach and iron powder reducing: measure clear water 2000ml with beaker and place water-bath, add vitriol oil 200ml, heat up and stir, slowly add in the beaker then calcining 460 grams and 46 gram manganese powders; When temperature rises to 95 ℃, be incubated 5 hours, add iron powder 70g, use the beaker sampling filtering; Filtrating is used the Rhocya titration again, and nondiscoloration is taken out overanxious; Get wet slag 112 grams, solution 2200ml, and sampling respectively
The result of laboratory test of slag is following:
| Element term | Zn％ | In(g/t) | Ag(g/t) | H 2O％ | Sn％ |
| Percentage composition | 1.54 | 213 | 2590 | 44.92 | 33.6 |
The result of laboratory test of solution is following:
| Element term | In(mg/l) | Zn(g/l) | H+(g/l) | Fe 3+(g/l) |
| Content | 292 | 47.17 | 101.52 | 0.4 |
Calculate: the leaching yield of Zn (in slag): 99%.The leaching yield of In (in slag) 98%; In 99% the Ag enrichment slag, in 90% the tin enrichment slag, the slag rate is 13.4%.
Indium is through extraction, and back extraction is replaced, and founding obtains 99% thick indium 628g, and direct yield has reached more than 94%.
Embodiment two:
Raw material: 500 tons of multi-metal tailings.Composition:
| Element term | Zn％ | In(g/t) | Ag(g/t) | Fe％ | Sn％ | H 2O％ | S％ |
| Percentage composition | 18～23 | 900～1500 | 300～450 | 20～25 | 4～5 | 6～10 | 19～23 |
| Average content | 22.5 | 1380 | 360 | 23 | 4.6 | 8 | 22 |
Manganese powder MO
2Greater than 55%
Sulfuric acid H
2SO
4Greater than 93%
Iron powder Fe is greater than 85%
1, disk pelletizing
After volume ratio is mixed at 3: 1 by weight with the vitriol oil with the low zinc multi-metal tailings of water content 6～8% high ferros, on the disk pelletizing machine, process the particle of 3-5mm size, tail gas entering exhaust treatment system
2, acidizing fired
To process the particulate material and evenly put into and carry out roasting in the rotary kiln, temperature is controlled at 400 ℃～650 ℃, 2～3 hours time; Flue gas gathers dust through surface cool device and pulsating collection device; Emptying after the ammonia process tail gas unit is handled again, calcining release grinding system is put into calcine bin.The collected ash of surface cool device and pulsating collection device reclaims other rare metals.
3, calcining ball milling
Calcining and flue dust are sent into dry ball, and vacuum is transported to calcine bin.
4, the hot acid of calcining leaches and iron powder reducing
At 50m
3The mechanical stirring reactive tank in, add the electrolysis waste solution of sulfuric acid and electrolytic zinc, guarantee sour 200g/L of beginning, liquid-solid ratio 5: 1 slowly adds time calcining 8t, adds manganese powder 80kg again, is warmed up to 90 ℃, behind the insulation 56h, analysis Fe
3+, calculate adding iron powder amount (iron content is greater than 88%), use the beaker sampling filtering, filtrating is used the Rhocya titration again, nondiscoloration, the notice press filtration obtains being rich in silver-colored scruff and contains indium, zinc, ferrous solution.Contain indium, zinc, ferrous solution and send the indium extraction, your smelting workshop section rich silver-colored scruff gives.
5, the extraction of indium
Contain indium, zinc, ferrous solution and send the indium extraction.Control condition: P
2O
4: 25%, thinner is a kerosene, extracts 8 grades, water: organic phase=6: 1, temperature 10-45 ℃.Raffinate returns the electrolytic zinc system; Back extraction: reverse-extraction agent is a hydrochloric acid, 3 grades of back extractions, water: organic phase=1: 15.
6, the displacement of indium
The solution of indium of back extraction is sent into displacement slot, replace, make indium be reduced to zeroth order, get the sponge indium with zinc metal sheet.
7, the founding of indium
Producing the sponge indium by the displacement operation and press group, send casting furnace to carry out founding, carry out electrolysis again, must purity be 99.99% electrolysis indium.
Raffinate returns the electrowinning zinc system, utilizes the patent No. ZL200810143744.3 of our company patent of invention raffinate to neutralize with secondary zinc oxide, and precipitating alum and removing iron purifies, electrodeposition, and founding obtains zinc ingot metal No. one.
Through 15 days commerical test, the thick indium 596.8kg of output 99%, a zinc metal sheet 99.36t, 65.6 tons of Fu Xiyin slags (butt).The direct yield 93% of indium, the direct yield 96% of zinc.
Silver scruff component list is following:
| Element term | Zn％ | In(g/t) | Ag(g/t) | H 2O％ | Sn％ |
| Percentage composition | 1.58 | 194 | 2490 | 28.6 | 29.2 |
Claims (1)
1. a method of from the low zinc multi-metal tailings of high ferro, extracting indium is characterized in that, may further comprise the steps:
1), disk pelletizing: after volume ratio is mixed at 3: 1 by weight with the vitriol oil with the low zinc multi-metal tailings of water content 6～8% high ferros, on the disk pelletizing machine, process the particle of 3-5mm size, tail gas entering exhaust treatment system;
2), acidizing fired: as will to process the particulate material and evenly put into and carry out roasting in the rotary kiln; Temperature is controlled at 400 ℃～650 ℃, and 2～3 hours time, flue gas gathers dust through surface cool device and pulsating collection device; Emptying after the ammonia process tail gas unit is handled again; Calcining release grinding system is put into calcine bin, and the collected ash of surface cool device and pulsating collection device reclaims other rare metals;
3), the hot acid of calcining leaches and the reduction of iron: the calcining that will pass through behind the ball milling adds in initial acid 180～200g/L sulphuric acid soln; Liquid-solid ratio 5-6: 1; 85～90 ℃ of temperature are incubated 5～6 hours, in temperature-rise period, add the pyrolusite of 8～10% calcining weight; Before the press filtration, analyze Fe3+, calculate the iron powder amount (iron content is greater than 88%) that adds, sampling filtering, filtrating is used the Rhocya titration again, nondiscoloration, press filtration obtains being rich in silver-colored scruff and contains indium, zinc, ferrous solution.Contain indium, zinc, ferrous solution and send the indium extraction, rich silver-colored scruff is managed elsewhere;
4), the extraction of indium: 25% P is adopted in extraction
2O
4, thinner is a kerosene, extracts 8 grades; Water: organic phase=6: 1, temperature 10-45 ℃, raffinate returns the electrolytic zinc system; The reverse-extraction agent that back extraction is adopted is a hydrochloric acid, 3 grades of back extractions; Water: organic phase=1: 15;
5), the solution of indium of back extraction is sent into displacement slot, replace, make indium be reduced to zeroth order with zinc metal sheet, the sponge indium;
6), the founding of indium: producing the sponge indium by the displacement operation and press group, send casting furnace to carry out founding, carry out electrolysis again, must purity be 99.99% electrolysis indium.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100405225A CN102560157A (en) | 2012-02-22 | 2012-02-22 | Method for reclaiming zinc and indium from high-iron low-zinc multi-metal tailings |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100405225A CN102560157A (en) | 2012-02-22 | 2012-02-22 | Method for reclaiming zinc and indium from high-iron low-zinc multi-metal tailings |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102787241A (en) * | 2012-09-10 | 2012-11-21 | 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 |
| CN104226461A (en) * | 2014-07-23 | 2014-12-24 | 紫金矿业集团股份有限公司 | Ore dressing method for comprehensively recovering gold, zinc, sulfur and iron from abandoned tailing |
| CN106337134A (en) * | 2016-09-30 | 2017-01-18 | 西安建筑科技大学 | Technique for recovering indium from indium-containing soot |
| CN107988486A (en) * | 2017-12-08 | 2018-05-04 | 江西自立环保科技有限公司 | A kind of method that zinc is recycled in the cigarette ash from fuming furnace |
| CN111286600A (en) * | 2018-12-06 | 2020-06-16 | 有研工程技术研究院有限公司 | Method for efficiently recovering zinc and iron from zinc ferrite-containing material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272553A (en) * | 1999-05-04 | 2000-11-08 | 沈奕林 | New process for recovering metals of indium, iron, silver and tin from high-indium high-iron zinc preparation concentrate |
| CN102312083A (en) * | 2011-09-23 | 2012-01-11 | 来宾华锡冶炼有限公司 | Method for extracting zinc indium and recovering iron from high-iron high indium zinc concentrate |
-
2012
- 2012-02-22 CN CN2012100405225A patent/CN102560157A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272553A (en) * | 1999-05-04 | 2000-11-08 | 沈奕林 | New process for recovering metals of indium, iron, silver and tin from high-indium high-iron zinc preparation concentrate |
| CN102312083A (en) * | 2011-09-23 | 2012-01-11 | 来宾华锡冶炼有限公司 | Method for extracting zinc indium and recovering iron from high-iron high indium zinc concentrate |
Non-Patent Citations (2)
| Title |
|---|
| 张瑜: "锌精矿制粒沸腾焙烧新工艺的应用与改进", 《有色金属（冶炼部分）》, no. 4, 31 August 2003 (2003-08-31), pages 18 - 19 * |
| 曹应科: "从铜冶炼砷烟灰中回收铟", 《湖南有色金属》, vol. 21, no. 1, 28 February 2005 (2005-02-28), pages 5 - 8 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102787241A (en) * | 2012-09-10 | 2012-11-21 | 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 |
| 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 |
| CN104226461A (en) * | 2014-07-23 | 2014-12-24 | 紫金矿业集团股份有限公司 | Ore dressing method for comprehensively recovering gold, zinc, sulfur and iron from abandoned tailing |
| CN106337134A (en) * | 2016-09-30 | 2017-01-18 | 西安建筑科技大学 | Technique for recovering indium from indium-containing soot |
| CN107988486A (en) * | 2017-12-08 | 2018-05-04 | 江西自立环保科技有限公司 | A kind of method that zinc is recycled in the cigarette ash from fuming furnace |
| CN111286600A (en) * | 2018-12-06 | 2020-06-16 | 有研工程技术研究院有限公司 | Method for efficiently recovering zinc and iron from zinc ferrite-containing material |
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Application publication date: 20120711 |