CN103643036A - Method for processing roasted sand containing iron, indium and zinc through hot-pressing selective leaching - Google Patents
Method for processing roasted sand containing iron, indium and zinc through hot-pressing selective leaching Download PDFInfo
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- CN103643036A CN103643036A CN201310719825.4A CN201310719825A CN103643036A CN 103643036 A CN103643036 A CN 103643036A CN 201310719825 A CN201310719825 A CN 201310719825A CN 103643036 A CN103643036 A CN 103643036A
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Abstract
The invention discloses a method of processing a material containing iron, indium and zinc through hot-pressing selective leaching. According to the method, ferric iron in zinc roasted sand is converted into ferrous iron by using reducing roasting; hot-pressing acidic selective leaching is carried out on reduced roasted sand in a autoclave; zinc and indium elements are leached out under high-temperature acidity condition and enter into a solution; since the pH value of the iron becomes negative in the case of hydrolysis in a high-temperature environment, iron is converted into hematite to be retained in leaching residue; leaching liquid is pre-neutralized and precipitates out indium, thus obtaining a zinc sulfate solution and indium residue; neutralization residues return to a rotary kiln to be subjected to reducing roasting together with the zinc roasted sand. By adopting the method, selective leaching of zinc, indium and iron of the roasted sand containing zinc, indium and iron is realized when the roasted sand is leached; the leaching rate of the indium is improved, and the cost of extracting the indium in the zinc roasted sand is reduced. The amount of powdered coal needed in the reducing roasting of the roasted sand is small, and the reducing atmosphere in a reducing roasting process is easily realized. The method can be applied to treatment of indium, zinc and other iron-containing non-ferrous metal materials.
Description
Technical field
The present invention relates to a kind of method that hot pressing selective leaching goes out to process iron content indium zinc baking sand, belong to technical field of wet metallurgy.
Background technology
Raw material be mainly derived from Guangxi, Yunnan, mining area, Hunan containing indium high ferro zinc baking sand, main component is: Zn42～52%, Fe10～20%, In500～1000g/t.In order to adapt in zinc baking sand, iron level is high, the costly feature of indium, considers the comprehensive utilization of association indium in zinc baking sand, and the technical process that zinc extracts is: neutral leaching, and low Ore Leaching, hot acid leaches, and siderotil method is sunk iron, indium etc.Iron vitriol slag is carried indium and is adopted rotary kiln evaporation, leaches extraction, displacement, the production technique of electrolysis.At present, there is following problem in this technique: (1) zinc, indium recovery are low, zinc recovery 92%, and indium recovery 70%, in addition, in concentrate, iron utilizes difficulty; (2) adopt hot acid to leach, the deironing of siderotil method, the iron vitriol slag of generation need reclaim zinc, indium through rotary kiln evaporation, and technical process is tediously long, and production cost is high, and off gas treatment amount is large.
Hot pressing leaching-out technique is successfully applied to the industrial production of zinc ore concentrate in the eighties in 20th century, make the simple of flowsheet of wet zinc smelting change, zinc sulphide in zinc ore concentrate generates metal sulfate and elementary sulfur with oxygen effect in waste electrolyte or acidic solution, and oxidation of pyrite directly generates sulfate radical.The efficiency that zinc ore concentrate hot pressing is leached is high, and adaptability is good, compares with the method for other zinc metallurgy, in environmental protection and economic aspect, has very strong competitive capacity.
Hematite process is based on the molten balance pH value of the acid of Fe2O3 under high temperature and becomes negative, and Zn
2+, Ni
2+hydrolysis pH value also positive many, make it in acidic solution, also can make iron with Fe
2o
3precipitation and, and Zn
2+, Ni
2+, Cu
2+plasma is still retained in solution, realizes not adding neutralizing agent and making iron and zinc, nickel, cobalt separated.
Summary of the invention
The object of this invention is to provide a kind of method that hot pressing selective leaching goes out to process iron content indium zinc baking sand, after iron indium zinc baking sand is mixed with coal dust batching, from chute, entering equipment raises the rotary kiln of plate structure, zinc baking sand is heated reduction in rotary kiln, by reducing roasting, the zinc ferrite in zinc baking sand is decomposed, ferric iron in calcining changes ferrous iron into, after reduced calcine mixes with waste electrolyte, in autoclave, hot pressing selectivity leaches, in calcining, zinc, indium leach and enter solution, and iron is suppressed to be retained in slag.Leach liquor regulates pH value by flue dust, oxide powder and zinc, indium hydrolytic precipitation, and solution of zinc sulfate send purifying electrolysis.
The present invention achieves the above object by the following technical programs: a kind of hot pressing selective leaching goes out to process the method for iron content indium zinc baking sand, comprises the following steps:
Step 1: by the zinc containing 42～52%, the zinc baking sand coal reduction of 10～20% iron, 0.050～0.1% indium, reduction apparatus is the built-in plate rotary kiln of raising, and destroys the structure of zinc ferrite in zinc baking sand by reducing roasting, in calcining, ferric iron is converted into ferrous iron; Control condition is: 700～900 ℃ of reduction temperatures, zinc baking sand contacts reduction, coal dust usage quantity 5～30%, kiln atmosphere CO concentration 1～10% in rotary kiln with coal dust, recovery time is controlled at 30min～90min, and the ferric reduction ratio of reduced calcine obtaining is 30～100%;
Step 2: the reduced calcine after reducing roasting is mixed and sized mixing with the sulphuric acid soln of 100～200g/L, and the quality of the sulphuric acid soln of the use of sizing mixing is 3～6 times of reduced calcine quality, obtains a kind of mixed slurry;
Step 3: described mixed slurry is added to autoclave, under being 160 ℃～200 ℃, the high temperature and high pressure environment of oxygen partial pressure 0.1～0.4MPa, temperature passes into oxygen, 2～4 hours reaction times, zinc in reduced calcine, indium leach and enter solution, iron in reduced calcine is converted into rhombohedral iron ore becomes scum, and the solution filter that reaction finishes obtains leach liquor and rhombohedral iron ore slag;
Step 4: leach liquor adds flue dust pre-neutralization pH0.5～1.5 to terminal, during Filter Press obtains and slag and pre-neutralization liquid, in and slag return in reduction rotary kiln and carry out reducing roasting;
Step 5: pre-neutralization liquid adds in oxide powder and zinc and heavy indium pH4.0～5.0 to terminal, and indium hydrolytic precipitation obtains heavy indium slag and heavy indium liquid, heavy indium slag is as the raw material of carrying indium, heavy indium liquid send to zinc sulfate cleaning section and purify after as the solution of zinc electrolysis.
The outstanding technique effect of the present invention is:
Adopting rotary kiln reducing roasting to process zinc baking sand needs coal amount few, and the reducing atmosphere that reduction needs is easily realized.
Adopt the acid selectivity of autoclave hot pressing to leach, extraction time is short, realizes zinc, indium and iron separated when leaching, and leaching yield is high, and scum is of high grade, the quantity of slag is few.
Adopt fluidized bed boiler has as the neutralizing agent of deironing liquid, adopt zinc oxide as the neutralizing agent of heavy indium, raw material sources are simple.Indium in zinc roasting obtains enrichment, can be used as the raw material reduction indium production cost of directly carrying indium.
All technical is good, leaching yield: Zn98.9%, Fe6.4%, In91.4%, scum rate 34.3%, scum grade 51.75%, heavy indium rate: 99.7%.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that hot pressing selective leaching of the present invention goes out to process the method for iron content indium zinc baking sand.
Embodiment
Embodiment 1
Hot pressing selective leaching of the present invention goes out to process the first example of the method for iron content indium zinc baking sand, comprises the steps:
Raw material: somewhere, Guangxi is containing Zn52.1%, Fe19.41%, the high ferro indium zinc baking sand of In0.057%.
Step 1: 900 ℃ of kiln temperatures, zinc baking sand is sneaked into 10% coal dust, adds in airtight rotary kiln, in kiln, install and raise plate, material rotates 75min discharging in kiln, and material drops to below 100 ℃ at identical reducing atmosphere, obtain reducing zinc baking sand, ferric iron is reduced to ferrous iron and reaches 92.6%.
Step 2: the reduced calcine obtaining mixes with acidic solution, the sulfuric acid content of acidic solution is 160g/L, and dropping into the quality of reduced calcine and the mass ratio of acidic solution is 1:6, and both add in autoclave after stirring.
Step 3: mixed solution carries out the leaching of hot pressing selectivity in autoclave, 195 ℃ of temperature of reaction, oxygen partial pressure 0.4MPa, 2 hours reaction times, after reaction finishes, carry out liquid-solid separation, obtain leach liquor and leached mud.Leaching yield: Zn98.6%, Fe6.4%, In91.5%.Scum productive rate 34.3%, iron grade 51.8% in scum, Zn1.45%.In leach liquor, Fe content is 1.9g/L, sulfuric acid content 37.1g/L.
Step 4: leach liquor adopts Zn dust to carry out pre-neutralization, and terminal is pH value 1.0, flue dust consumption (to zinc baking sand mass ratio) 40.7%, in slag rate 18.8%.
Step 5: regulate the pH value to 4.5 of pre-neutralization liquid with oxide powder and zinc, oxide powder and zinc consumption 13.8%, obtains heavy indium slag, slag rate 4.8%, indium slag, containing indium 1.86%, contains zinc 36.8%, iron content 12.4%, liquid iron 0.016g/L after heavy indium.
Embodiment 2
Hot pressing selective leaching of the present invention goes out to process another example of the method for iron content indium zinc baking sand, comprises the steps:
Raw material: calcining is containing Zn43.8%, Fe22.9%, In0.078%.
Step 1: adopt rotary kiln reduction zinc baking sand, 800 ℃ of kiln temperatures, go back raw coal amount 15%, reduction 90min, the reduced calcine of ferric iron reduction ratio 93.8%.
Step 2: reduced calcine and acid solution are sized mixing, acid solution sulfur acid 180, solid-liquid mass ratio is 1:6, after mixing, adds autoclave.
Step 3: reduced calcine carries out the leaching of hot pressing selectivity in autoclave, leaching yield: Zn98.9%, Fe8.6%, In94.2% obtain scum 32.8%, the grade 56.1% of iron in scum.
Step 4: flue dust pre-neutralization, pre-neutralization terminal 1.5, flue dust consumption 46.2%, pre neutralization dreg rate 22.1%.
Step 5: oxide powder and zinc sinks indium, endpoint pH 5.0, oxide powder and zinc consumption 10.5%, obtains heavy indium slag, slag rate 4.2%, indium slag is containing indium 3.1%, liquid iron level 0.008g/L after heavy indium.
Embodiment 3
Hot pressing selective leaching of the present invention goes out to process another example of the method for iron content indium zinc baking sand, comprises the steps:
Raw material: calcining is containing Zn46.0%, Fe18.02%, In0.049%.
Step 1: adopt rotary kiln reduction zinc baking sand, go back raw coal amount 8%, 850 ℃ of reduction temperatures, reduction 45min, obtains the reduced calcine of reduction ratio 82.5%.
Step 2: reduced calcine and acid solution are sized mixing, acid solution sulfur acid 180g/L, solid-liquid mass ratio is 1:5, after mixing, adds autoclave.
Step 3: reduced calcine carries out the leaching of hot pressing selectivity in autoclave, 180 ℃ of hot pressure reaction temperature, reaction pressure 1.6Mpa, leach liquor is containing zinc 83.7g/L, indium 67mg/L, iron 0.62g/L, leaching yield is Zn98.8%, In83.2%, Fe1.91%, obtains scum 38.7%, the grade 50.9% of iron in scum.
Step 4: flue dust pre-neutralization, pre-neutralization terminal 1.5, flue dust consumption 46.2%, pre neutralization dreg rate 22.1%.
Step 5: oxide powder and zinc sinks indium, oxide powder and zinc consumption 9.3%, obtains heavy indium slag, slag rate 3.92%, indium slag is containing indium 2.23%, and containing zinc 37.08%, iron content 10.5%, after heavy indium, liquid iron is lower than 0.018g/L.
Claims (2)
1. hot pressing selective leaching goes out to process a method for iron content indium zinc baking sand, it is characterized in that, comprises the following steps:
Step 1: by the zinc containing 42～52%, the zinc baking sand coal reduction of 10～20% iron, 0.050～0.1% indium, reduction apparatus is the built-in plate rotary kiln of raising, and destroys the structure of zinc ferrite in zinc baking sand by reducing roasting, in calcining, ferric iron is converted into ferrous iron; Control condition is: 700～900 ℃ of reduction temperatures, zinc baking sand contacts reduction, coal dust usage quantity 5～30%, kiln atmosphere CO concentration 1～10% in rotary kiln with coal dust, recovery time is controlled at 30min～90min, and the ferric reduction ratio of reduced calcine obtaining is 30～100%;
Step 2: the reduced calcine after reducing roasting is mixed and sized mixing with the sulphuric acid soln of 100～200g/L, and the quality of the sulphuric acid soln of the use of sizing mixing is 3～6 times of reduced calcine quality, obtains a kind of mixed slurry;
Step 3: described mixed slurry is added to autoclave, under being 160 ℃～200 ℃, the high temperature and high pressure environment of oxygen partial pressure 0.1～0.4MPa, temperature passes into oxygen, 2～4 hours reaction times, zinc in reduced calcine, indium leach and enter solution, iron in reduced calcine is converted into rhombohedral iron ore becomes scum, and the solution filter that reaction finishes obtains leach liquor and rhombohedral iron ore slag;
Step 4: leach liquor adds flue dust pre-neutralization pH0.5～1.5 to terminal, during Filter Press obtains and slag and pre-neutralization liquid, in and slag return in reduction rotary kiln and carry out reducing roasting;
Step 5: pre-neutralization liquid adds in oxide powder and zinc and heavy indium pH4.0～5.0 to terminal, and indium hydrolytic precipitation obtains heavy indium slag and heavy indium liquid, heavy indium slag is as the raw material of carrying indium, heavy indium liquid send to zinc sulfate cleaning section and purify after as the solution of zinc electrolysis.
2. hot pressing selective leaching according to claim 1 goes out to process the method for iron content indium zinc baking sand, it is characterized in that, it is after a circulation that mixing in described step 2 is sized mixing, with zinc electrolysis waste solution, mix and size mixing, zinc electrolysis waste solution sulfur acid 100～200g/L, the quality of the zinc electrolysis waste solution of the use of sizing mixing is 3～6 times of reduced calcine quality, and the sulfuric acid quality in solution is the quality 0.8～1.4 of reduced calcine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310719825.4A CN103643036A (en) | 2013-12-20 | 2013-12-20 | Method for processing roasted sand containing iron, indium and zinc through hot-pressing selective leaching |
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| CN201310719825.4A CN103643036A (en) | 2013-12-20 | 2013-12-20 | Method for processing roasted sand containing iron, indium and zinc through hot-pressing selective leaching |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834755A (en) * | 2016-12-28 | 2017-06-13 | 呼伦贝尔驰宏矿业有限公司 | A kind of technique of the concentration and separation of oxygen leaching liquid containing indium indium |
| US20190233302A1 (en) * | 2018-02-01 | 2019-08-01 | Korea Zinc Co., Ltd. | Method of recovering iron from zinc sulphate solution |
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| 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 |
| CN102560087A (en) * | 2012-03-23 | 2012-07-11 | 广西冶金研究院 | Method for extracting indium and zinc from high-iron indium-containing zinc calcine and preparing iron oxide |
| WO2012140284A1 (en) * | 2011-04-15 | 2012-10-18 | Tam 5, S.L. | Hydrometallurgical method for the recovery of zinc in a sulphur medium from sulphured zinc concentrates |
| CN103409621A (en) * | 2013-07-22 | 2013-11-27 | 昆明理工大学科技产业经营管理有限公司 | Combined leaching method for high-iron zinc sulfide concentrate and high-iron zinc calcine leaching slag |
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2013
- 2013-12-20 CN CN201310719825.4A patent/CN103643036A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012140284A1 (en) * | 2011-04-15 | 2012-10-18 | Tam 5, S.L. | Hydrometallurgical method for the recovery of zinc in a sulphur medium from sulphured zinc concentrates |
| 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 |
| CN102560087A (en) * | 2012-03-23 | 2012-07-11 | 广西冶金研究院 | Method for extracting indium and zinc from high-iron indium-containing zinc calcine and preparing iron oxide |
| CN103409621A (en) * | 2013-07-22 | 2013-11-27 | 昆明理工大学科技产业经营管理有限公司 | Combined leaching method for high-iron zinc sulfide concentrate and high-iron zinc calcine leaching slag |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834755A (en) * | 2016-12-28 | 2017-06-13 | 呼伦贝尔驰宏矿业有限公司 | A kind of technique of the concentration and separation of oxygen leaching liquid containing indium indium |
| US20190233302A1 (en) * | 2018-02-01 | 2019-08-01 | Korea Zinc Co., Ltd. | Method of recovering iron from zinc sulphate solution |
| US11001507B2 (en) * | 2018-02-01 | 2021-05-11 | Korea Zinc Co., Ltd. | Method of recovering iron from zinc sulphate solution |
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Application publication date: 20140319 |