CN102560087B - Method for extracting indium and zinc from high-iron indium-containing zinc calcine and preparing iron oxide - Google Patents
Method for extracting indium and zinc from high-iron indium-containing zinc calcine and preparing iron oxide Download PDFInfo
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Abstract
The invention relates to a method for extracting indium and zinc from high-iron indium-containing zinc calcine and preparing iron oxide. A zinc ferrite structure in the high-iron indium-containing zinc calcine is damaged by reduction roasting, elements such as zinc, iron and indium in the reduced calcine are obtained by neutral leaching and acid leaching, indium-rich slag is obtained by neutralization for precipitating indium, the iron grade of slag obtained by removing iron from hematite under high pressure is high, an industrial iron oxide product can be obtained by acid washing and roasting, and liquid obtained after the iron is removed can be directly purified and electrolyzed after being neutralized by smoke. A technical route of maximally extracting base metal such as the indium, the zinc and the like and recycling associated iron minerals simultaneously is provided, and the problems that the recovery rate of the indium is low and the iron cannot be recycled in the process of smelting a high-iron indium-containing zinc concentrate at present are solved; and a clean production technology which combines effective extraction of the base metal with effective utilization of associated iron is provided for treating the indium, the zinc and other high-iron non-ferrous metal materials.
Description
Technical field
The present invention relates to a kind of method of extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand, belong to technical field of mineral processing.
Background technology
China's zinc smeltery has early carried out hot acid leaching-jarosite process, goethite process, hematite process, spray except the Test And Research Work of the techniques such as iron processes, except hematite process is subjected to the device fabrication horizontal constraints, during other several techniques all have been applied to produce.Adopt hot acid leaching-jarosite process as smeltery, silver northwest, the smeltery, Chifeng adopts the ammonium alum iron processes, and smeltery, Wenzhou adopts spray to remove iron processes etc.The leaching yield of hot acid extract technology is high, can obtain to contain zinc, plumbous silver-colored slag that indium is low, but iron vitriol slag content has soluble ion, easily causes environmental pollution, simultaneously the recovery difficulty of the associated metal such as indium.
For main component be: Zn46～52%, Fe14～18%, In800～1400g/t, S28～30% contain the indium high-iron zinc sulfide concentrate.Present technical process is hot acid leaching-ihleite method: fluidized bed roasting, and neutral the leaching, low Ore Leaching, hot acid leaches, and the ammonium iron alum method sink iron, indium, and iron vitriol slag is carried indium and is adopted rotary kiln evaporation, leaches, and the production technique of electrolysis is replaced in extraction.There is following problem in this technique: (1) zinc, indium recovery are low, zinc recovery 88.2%, 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 needs to reclaim zinc, indium through rotary kiln evaporation, and technical process is tediously long, and production cost is high, and the off gas treatment amount is large.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand, adopt the method can simplify indium, zinc extraction metallurgical technology flow process, significantly improve the smelting recovery of indium, zinc, indium recovery reaches 90%, zinc recovery reaches 98%, and makes that in mineral, the iron of association is utilized effectively.Solve the problem that in present high ferro Indium-Zinc concentrate smelting process, indium recovery is low, iron can not get recycling.
The present invention achieves the above object by the following technical programs: a kind of method of extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand comprises the following steps:
1, will contain 46～54% zinc, the high ferro zinc baking sand of iron 16～20%, indium 0.074～0.093% contacts reduction with CO in rotary kiln, and reduction temperature is at 700～900 ℃, CO concentration 10～30%, coefficient of excess 0.8～3, the recovery time is controlled at 30～80min, obtains reduced calcine.
2, the reduced calcine that obtains is carried out neutrality with sulfuric acid and leaches, press liquid and solids ratios (volume/weight) and be 5:1, neutrally leach initial acidity 100～150g/L, terminal point pH 5.4, filtration obtain neutral leach liquor with in soak slag.
3, carry out acidic leaching with soaking slag in described, the initial acidity 160～200g/L of acidic leaching, 80～95 ℃ of extraction temperatures, acidic leaching terminal point acidity 10g～50g/L, extraction time 2～4 hours filters to get acid leaching solution and acidic leaching residue.
4, adopt in zinc oxide the acid leaching solution that obtains and heavy indium, liquid after heavy indium slag and heavy indium is filtered to get in the terminal point pH4 of heavy indium～4.8.
After the neutral leach liquor that 5, will obtain and heavy indium, liquid adds autoclave after mixing, pass into oxygen, at 160～200 ℃, keep oxygen partial pressure 0.2～0.4MPa, 2～4 hours deironing time, form hematite precipitation after making the ferrous iron oxidation in solution, filter and to obtain liquid and rhombohedral iron ore slag after deironing.
6, gained rhombohedral iron ore slag was with 0.2～1.5mol/L HCl stirring and pickling 0.5～2 hour, 30～80 ℃ of temperature, filter the rhombohedral iron ore obtain after pickling in 600～900 ℃ of roasting temperatures 0.5～1 hour, obtain meeting the brown iron oxide that HC/T2574-94 industrial ferric oxide II type requires.
7, after the gained deironing, liquid adopts the neutralization of fluidized bed roasting flue dust, in and terminal point pH5.4, after neutralizer purifies, electrodeposition obtains metallic zinc, in and the secondary zinc oxide that produces after reduction volatilization of slag as the neutralizing agent of the heavy indium of pickling liquor.
Described reduced calcine is at N
2Protection is lower cooling.
Know-why of the present invention is that the hot zinc baking sand of the oxidizing roasting of just having completed is put into rotary kiln, under the reductive action of CO, destroy the zinc ferrite structure in the zinc roasting, reduced calcine zinc, indium, iron when low Ore Leaching can be leached in a large number, and solution carries out the heavy indium of pre-neutralization, and heavy indium liquid enters autoclave and carries out the rhombohedral iron ore deironing, the further removal of impurities of scum is purified, product obtain respectively being rich in indium in and slag, secondary oxidation iron powder, liquid after the zinc deironing.
The reducing roasting principal reaction has: 3ZnFe
2O
4+ CO → 3ZnO+2Fe
3O
4+ CO
2
ZnFe
2O
4+CO→ZnO+2FeO+CO
2
Reach the purpose of decomposing zinc ferrite.
Outstanding substantive distinguishing features of the present invention and marked improvement are:
1, adopt reducing roasting to process zinc baking sand the leaching performance of Zn, In is significantly improved, leach index excellent.
2, adopt the hematite process deironing, scum is of high grade, the quantity of slag is few, be easy to recycling.
3, adopt fluidized bed boiler has as the neutralizing agent of deironing liquid, in and the oxide zinc with indium content that produces through volatilization of slag as the neutralizing agent of heavy indium, the indium in flue dust also obtains enrichment, has solved the problem that neutralizing agent needs outsourcing.
4, adopt the present invention to obtain technical indicator preferably: Zn leaching yield 99.03%, In leaching yield 92.86%, heavy indium rate 99.47%, deironing rate 98.29%, acid leaching residue rate 7.75%, scum rate 29.05%, scum grade 61.84%, industrial iron oxide product contains Fe
2O
397.65%.
Description of drawings
Fig. 1 is the process flow sheet that extracts indium zinc and prepare the method for ferric oxide from contain high ferro indium zinc baking sand of the present invention.
Embodiment
Below by specific embodiment, technical scheme of the present invention is further described.
Embodiment 1
The method of extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand of the present invention, carry out according to the following steps:
The high ferro zinc baking sand that 1, will contain Zn 53.54%, Fe 19.42%, In 0.092% contacts reduction with CO in rotary kiln, reduction temperature is at 870～900 ℃, pass into the nitrogen that contains 20% carbon monoxide, coefficient of excess 1.2, add high ferro indium zinc baking sand by 6kg/h, install in kiln and raise plate, material rotates the 30min discharging in kiln, material drops to room temperature at identical reducing atmosphere, obtains Fe
2+14.96% reduced calcine, its main chemical compositions is:
 |
Zn% | Fe% | Fe 2+% | In% | Reduction ratio % |
| Reduced calcine | 53.54 | 19.42 | 14.96 | 0.092 | 77.03 |
[0022]2, the reduced calcine that obtains is carried out neutrality with sulfuric acid according to a conventional method and leach, press liquid and solids ratios (volume/weight) and be 5:1, neutral initial acidity 150g/L, leaching 30min, the terminal point pH5.4 of leaching.Filtration obtain neutral leach liquor and in soak slag.The neutral leaching yield 86.34% that leaches Zn, iron 49.5%.
3, carry out acidic leaching with soaking slag in described, leach initial acidity 200g/L, 85 ℃ of extraction temperatures, time 2 h, pickling liquor is sour 45g/L eventually.Filtration obtains acid leaching solution and acidic leaching residue, the leaching yield 99.03% of acidic leaching Zn, iron 93.11%, indium 92.86%.
4, adopt in zinc oxide the acid leaching solution that obtains and heavy indium, zinc oxide dosage is 13.75% of calcining weight, heavy indium endpoint pH 4.5, and heavy indium rate 99.47% is filtered to get liquid after heavy indium slag and heavy indium.
After after the neutral leach liquor that 5, will obtain and heavy indium, liquid mixes, add and carry out the high pressure deironing in autoclave, pass into oxygen, 200 ℃ of deironing temperature, under oxygen partial pressure 0.2MPa, 4 hours deironing time, form hematite precipitation after making the ferrous iron oxidation in solution, filtration obtains liquid and rhombohedral iron ore slag after deironing, deironing rate 98.29%.The rhombohedral iron ore slag contains Fe61.84%, Zn1.45%, S1.98%.
6, described rhombohedral iron ore scum is used 0.5mol/L HCl agitator treating 30min, temperature 60 C, the rhombohedral iron ore that after pickling, filtration obtains is in the retort furnace roasting, 800 ℃ of maturing temperatures, roasting time 30min, obtain containing the brown iron oxide that meets HC/T2574-94 industrial ferric oxide II type requirement of ferric oxide 97.65%, productive rate 89.8%.In washings lime and rear qualified discharging.
7, liquid after described deironing is adopted the neutralization of fluidized bed roasting flue dust, in and terminal point pH5.4, after neutralizer purifies, electrodeposition obtains metallic zinc, in and the secondary zinc oxide that produces after reduction volatilization of slag as the neutralizing agent of the heavy indium of pickling liquor.
Embodiment 2
A kind of method of extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand comprises the following steps:
1, will contain Zn50.9%, Fe20.81%, the high ferro indium zinc baking sand of In0.10% contacts reduction with CO in rotary kiln, pass into the nitrogen that contains 10% carbon monoxide, coefficient of excess 0.8,770～800 ℃ of reduction temperatures, recovery time 80min obtains containing Fe
2+13.88% reduced calcine, reduction ratio 66.7%.
2, the reduced calcine that obtains being carried out neutrality with sulfuric acid leaches, the initial acidity 120g/L of neutral leaching, liquid and solids ratios (volume/weight) are 5:1, the neutral terminal point pH 5.4 that leaches, neutral extraction time 30 min, filtration obtain neutral leach liquor and in soak slag, neutral leaching yield Zn75.9%, the Fe53.3% of leaching.
3, carry out acidic leaching with soaking slag in described, the initial acidity 160g/L of acidic leaching, 95 ℃ of extraction temperatures, acidic leaching terminal point acidity 10g/L, extraction time 4 hours filters and obtains acid leaching solution and acidic leaching residue, the leaching yield Zn99.0% of acidic leaching, Fe91.8%, In90.7%.
4, adopt in zinc oxide the acid leaching solution that obtains and heavy indium, the terminal point pH4.0 of heavy indium filters to get liquid after heavy indium slag and heavy indium, heavy indium rate 98.6%.
After after the neutral leach liquor that 5, will obtain and heavy indium, liquid mixes, add autoclave, pass into oxygen, at 190 ℃, keep oxygen partial pressure 0.3MPa, 3 hours deironing time, form hematite precipitation after making the ferrous iron oxidation in solution, filtration obtains liquid and rhombohedral iron ore slag after deironing, deironing rate 97.79%.The rhombohedral iron ore slag contains Fe61.77%, Zn1.52%, S1.82%.
6, gained rhombohedral iron ore slag 1mol/L HCl stirring and pickling 60min, 80 ℃ of temperature, the rhombohedral iron ore that after pickling, filtration obtains obtains containing ferric oxide 98.05% and meets the brown iron oxide that HC/T2574-94 industrial ferric oxide II type requires, productive rate 79.3% in 700 ℃ of roasting temperature 80min.
7, after the gained deironing, liquid adopts the neutralization of fluidized bed roasting flue dust, in and terminal point pH5.4, after neutralizer purifies, electrodeposition obtains metallic zinc, in and the secondary zinc oxide that produces after reduction volatilization of slag as the neutralizing agent of the heavy indium of pickling liquor.
Embodiment 3
A kind of method of extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand comprises the following steps:
1, will contain Zn53.2%, Fe18.98%, the high ferro zinc baking sand of In0.093% contact reduction with CO in rotary kiln, pass into the nitrogen that contains 30% carbon monoxide, coefficient of excess 2, and 700～730 ℃ of reduction temperatures, recovery time 60min obtains containing Fe
2+15.21% reduced calcine, reduction ratio 80.1%.
2, the reduced calcine that obtains is carried out neutrality with sulfuric acid and leach, the initial acidity 100g/L of neutral leaching, liquid and solids ratios (volume/weight) they are 5:1, terminal point pH 5.4, filtration obtain neutral leach liquor and in soak slag, the neutral leaching yield 69.38% that leaches Zn, iron 55.8%.
3, carry out acidic leaching with soaking slag in described, the initial acidity 200g/L of acidic leaching, 95 ℃ of extraction temperatures, acidic leaching terminal point acidity 50g/L, extraction time 2 hours filters and obtains acid leaching solution and acidic leaching residue, the leaching yield Zn99.7% of acidic leaching, Fe95.8%, In92.3%.
4, adopt in zinc oxide the acid leaching solution that obtains and heavy indium, the terminal point pH4.8 of heavy indium filters to get liquid after heavy indium slag and heavy indium, heavy indium rate 99.9%.
After the neutral leach liquor that 5, will obtain and heavy indium, liquid adds autoclave after mixing, pass into oxygen, at 170 ℃, keep oxygen partial pressure 0.4MPa, the deironing time 2 h, form hematite precipitation after making the ferrous iron oxidation in solution, filter liquid and rhombohedral iron ore slag after deironing, the deironing rate 95.69% of obtaining.The rhombohedral iron ore slag contains Fe59.86%, Zn1.59%, S2.17%.
6, gained rhombohedral iron ore slag is used 1mol/L HCl stirring and pickling 1.5 hours, temperature 70 C, filter the rhombohedral iron ore obtain after pickling in 850 ℃ of roasting temperatures 1 hour, what obtain containing ferric oxide 97.22% meets the brown iron oxide that HC/T2574-94 industrial ferric oxide II type requires, productive rate 76.9%.
7, after the gained deironing, liquid adopts the neutralization of fluidized bed roasting flue dust, in and terminal point pH5.4, after neutralizer purifies, electrodeposition obtains metallic zinc, in and the secondary zinc oxide that produces after reduction volatilization of slag as the neutralizing agent of the heavy indium of pickling liquor.
Embodiment 4
A kind of method of extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand comprises the following steps:
1, will contain Zn51.7%, Fe21.02%, the high ferro zinc baking sand of In0.096% contact reduction with CO in rotary kiln, pass into the nitrogen that contains 20% carbon monoxide, coefficient of excess 3, and 800～830 ℃ of reduction temperatures, recovery time 100min obtains containing Fe
2+16.51% reduced calcine, reduction ratio 78.54%.
2, the reduced calcine that obtains is carried out neutrality with sulfuric acid and leach, the initial acidity 150g/L of neutral leaching, liquid and solids ratios (volume/weight) they are 5:1, terminal point pH 5.4, filtration obtain neutral leach liquor and in soak slag, the neutral leaching yield 84.64% that leaches Zn, iron 49.83%.
3, carry out acidic leaching with soaking slag in described, the initial acidity 180g/L of acidic leaching, 80 ℃ of extraction temperatures, acidic leaching terminal point acidity 28g/L, extraction time 4 hours filters and obtains acid leaching solution and acidic leaching residue, the leaching yield Zn99.1% of acidic leaching, Fe94.4%, In91.6%.
4, adopt in zinc oxide the acid leaching solution that obtains and heavy indium, the terminal point pH4.6 of heavy indium filters to get liquid after heavy indium slag and heavy indium, heavy indium rate 99.5%.
After the neutral leach liquor that 5, will obtain and heavy indium, liquid adds autoclave after mixing, pass into oxygen, at 160 ℃, keep oxygen partial pressure 0.4MPa, 4 hours deironing time, form hematite precipitation after making the ferrous iron oxidation in solution, filter liquid and rhombohedral iron ore slag after deironing, the deironing rate 94.75% of obtaining.The rhombohedral iron ore slag contains Fe59.76%, Zn1.84%, S2.02%.
6, gained rhombohedral iron ore slag is used 1mol/L HCl stirring and pickling 1.5 hours, 30 ℃ of temperature, filter the rhombohedral iron ore obtain after pickling in 850 ℃ of roasting temperatures 1 hour, what obtain containing ferric oxide 96.05% meets the brown iron oxide that HC/T2574-94 industrial ferric oxide II type requires, productive rate 75.8%.
7, after the gained deironing, liquid adopts the neutralization of fluidized bed roasting flue dust, in and terminal point pH5.4, after neutralizer purifies, electrodeposition obtains metallic zinc, in and the secondary zinc oxide that produces after reduction volatilization of slag as the neutralizing agent of the heavy indium of pickling liquor.
Claims (2)
1. the method extracting indium zinc and prepare ferric oxide from contain high ferro indium zinc baking sand, is characterized in that, the method comprises the following steps:
1.1 will contain 46～54% zinc, the high ferro indium zinc baking sand of iron 16～20%, indium 0.074～0.100% contacts reduction with CO in rotary kiln, reduction temperature is at 700～900 ℃, CO concentration 10～30%, coefficient of excess 0.8～3, the recovery time is controlled at 30～100min, obtain reduced calcine
Leach 1.2 the reduced calcine that obtains is carried out neutrality with sulfuric acid, press liquid and solids ratios (volume/weight) and be 5:1, neutrally leach initial acidity 100～150g/L, the neutral terminal point pH5.4 that leaches, filtration obtain neutral leach liquor with in soak slag,
1.3 carry out acidic leaching with soaking slag in described, the initial acidity 160～200g/L of acidic leaching, 80～95 ℃ of extraction temperatures, acidic leaching terminal point acidity 10～50g/L, extraction time 2～4 hours filters to get acid leaching solution and acidic leaching residue,
1.4 adopt in zinc oxide the acid leaching solution that obtains and heavy indium, liquid after heavy indium slag and heavy indium is filtered to get in the terminal point pH4 of heavy indium～4.8,
1.5 after the neutral leach liquor that will obtain and heavy indium, liquid adds autoclave after mixing, and passes into oxygen, at 160～200 ℃, keep oxygen partial pressure 0.2～0.4MPa, 2～4 hours deironing time, form hematite precipitation after making the ferrous iron oxidation in solution, filtration obtains liquid and rhombohedral iron ore slag after deironing
1.6 gained rhombohedral iron ore slag was with 0.2～1.5mol/L HCl stirring and pickling 0.5～2 hour, 30～90 ℃ of temperature, filter the rhombohedral iron ore obtain after pickling in 600～900 ℃ of roasting temperatures 0.5～1 hour, obtain meeting the brown iron oxide that HC/T2574-94 industrial ferric oxide II type requires
1.7 after the gained deironing, liquid adopts the neutralization of fluidized bed roasting flue dust, in and terminal point pH5.4, after neutralizer purifies, electrodeposition obtains metallic zinc, in and the secondary zinc oxide that produces after reduction volatilization of slag as the neutralizing agent of the heavy indium of pickling liquor.
2. the method for extracting indium zinc and prepare ferric oxide from containing high ferro indium zinc baking sand according to claim 1, is characterized in that, described reduced calcine is at N
2Protection is lower cooling.
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| MX349844B (en) * | 2012-07-16 | 2017-08-16 | Tam 5 S L * | Hydrometallurgical method for recovering zinc in a sulphuric medium from zinc sulphide concentrates having a high iron content. |
| CN102776384A (en) * | 2012-08-08 | 2012-11-14 | 汉源县广超有色金属综合回收有限责任公司 | Method for extracting zinc from non-ferrous metal waste residue |
| CN103173625B (en) * | 2013-04-19 | 2014-12-10 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
| CN103276197B (en) * | 2013-05-17 | 2015-04-08 | 中南大学 | Method for performing flash reducing and roasting on zinc calcine |
| CN103643036A (en) * | 2013-12-20 | 2014-03-19 | 广西冶金研究院 | Method for processing roasted sand containing iron, indium and zinc through hot-pressing selective leaching |
| CN104141046B (en) * | 2014-07-24 | 2016-10-05 | 安阳市岷山有色金属有限责任公司 | A kind of method that indium zinc recovering is carried out to oxide zinc with indium content cigarette ash |
| 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 |
| CN104561610B (en) * | 2014-12-26 | 2017-04-12 | 河南豫光锌业有限公司 | Method and device for treating washing water in refined indium production |
| CN105603210B (en) * | 2016-03-11 | 2018-08-07 | 北京科技大学 | A kind of short route pyrometallurgy of zinc method |
| CN106868304A (en) * | 2016-12-27 | 2017-06-20 | 河南豫光锌业有限公司 | A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum |
| CN108728667A (en) * | 2018-05-29 | 2018-11-02 | 南丹县南方有色金属有限责任公司 | A kind of method that oxygen removes iron |
| CN110295290B (en) * | 2019-07-08 | 2021-06-01 | 云南驰宏资源综合利用有限公司 | Method for leaching zinc by acid leaching slag and lead slag in one-kettle three-stage oxygen pressure manner |
| CN111206155B (en) * | 2020-02-28 | 2021-08-27 | 白银有色集团股份有限公司 | Method for recovering zinc metal by using regenerated zinc oxide |
| CN112522520A (en) * | 2020-12-02 | 2021-03-19 | 陕西锌业有限公司 | Method for directly producing electrolytic zinc by using secondary zinc oxide |
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