CN102560087A - 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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- CN102560087A CN102560087A CN2012100785686A CN201210078568A CN102560087A CN 102560087 A CN102560087 A CN 102560087A CN 2012100785686 A CN2012100785686 A CN 2012100785686A CN 201210078568 A CN201210078568 A CN 201210078568A CN 102560087 A CN102560087 A CN 102560087A
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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 from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone, belong to technical field of mineral processing.
Background technology
China zinc smeltery has early carried out the experimental study work that hot acid leaching-jarosite process, goethite process, hematite process, spray remove technologies such as iron processes, except that hematite process receives the device fabrication horizontal constraints, during other several kinds of technologies all have been applied to produce.Adopt hot acid leaching-jarosite process like 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, is prone to cause environmental pollution, simultaneously the recovery difficulty of associated metal such as indium.
For staple be: Zn46～52%, Fe14～18%, In800～1400g/t, S28～30% contain the indium high-iron zinc sulfide concentrate.Present main technique flow process is a hot acid leaching-ihleite method: fluidized bed roasting, and neutral the leaching, low acidleach goes out, and 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 electrolytic production technique is replaced in extraction.There is following problem in this technology: (1) zinc, indium recovery are low, zinc recovery 88.2%, and indium recovery 70%, in addition, iron utilizes difficulty in the concentrate; (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 big.
Summary of the invention
The purpose of this invention is to provide a kind of method of from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone; Adopt this method can simplify indium, zinc extraction metallurgical technology flow process; Significantly improve the smelting recovery of indium, zinc; Indium recovery reaches 90%, and zinc recovery reaches 98%, and makes that the iron of association is utilized effectively in the mineral.Solve the problem that indium recovery is low, iron can not get recycling in the present high ferro indium zinc ore concentrate smelting process.
The present invention achieves the above object through following technical scheme: a kind of method of from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone may further comprise the 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 and in soak slag.
3, carry out acidity and leach soaking slag in said, acidly leach initial acidity 160～200g/L, 80～95 ℃ of extraction temperatures, the acid terminal point acidity 10g～50g/L that leaches, extraction time 2～4 hours is crossed and is filtered acid leaching solution and acid leached mud.
4, adopt in the zinc oxide acid leaching solution that obtains and heavy indium, terminal point pH4～4.8 of heavy indium are crossed and are filtered liquid behind heavy indium slag and the heavy indium.
Liquid mixes the back and adds autoclave behind neutral leach liquor that 5, will obtain and the heavy indium; Aerating oxygen; At 160～200 ℃, keep oxygen partial pressure 0.2～0.4MPa, 2～4 hours deironing time; Form hematite precipitation after making the oxidation of divalent in the solution, filter and to obtain liquid and rhombohedral iron ore slag after the 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; The rhombohedral iron ore that the pickling after-filtration obtains obtains meeting the brown iron oxide that the industrial red stone II of HC/T2574-94 type requires in 600～900 ℃ of roasting temperatures 0.5～1 hour.
7, liquid adopts the neutralization of fluidized bed roasting flue dust after the gained deironing, in terminal point pH5.4, neutralizer purifies the back electrodeposition and obtains metallic zinc, in the secondary zinc oxide that after reduction volatilization, produces with slag as the neutralizing agent of the heavy indium of pickling liquor.
Said reduced calcine is at N
2Protection cooling down.
Know-why of the present invention is to put into rotary kiln to the hot zinc baking sand of the oxidizing roasting of just having accomplished, and under the reductive action of CO, destroys the zinc ferrite structure in the zinc roasting; Reduced calcine zinc, indium, iron when low acidleach goes out can be leached in a large number, and solution carries out the heavy indium of pre-neutralization, and heavy indium liquid gets into 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 handle zinc baking sand the leaching performance of Zn, In is significantly improved, it is excellent to leach index.
2, adopt the hematite process deironing, scum is of high grade, the quantity of slag is few, be easy to recycling.
3, adopt the neutralizing agent of fluidized bed boiler has as deironing liquid, in contain the neutralizing agent of indium zinc oxide with slag through what volatilization produced as heavy indium, the indium in the 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 from contain high ferro indium zinc baking sand, extracts indium zinc and prepare the method for red stone of the present invention.
Embodiment
Below through specific embodiment technical scheme of the present invention is further described.
Embodiment 1
The method of from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone 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 feeds the nitrogen that contains 20% carbon monoxide at 870～900 ℃; Coefficient of excess 1.2; Press 6kg/h and add high ferro indium zinc baking sand, install in the 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 by ordinary method with sulfuric acid 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 with in soak slag.The neutral leaching yield 86.34% that leaches Zn, iron 49.5%.
3, carry out the acidity leaching with soaking slag in said, leach initial acidity 200g/L, 85 ℃ of extraction temperatures, 2 hours time, pickling liquor is sour 45g/L eventually.Filtration obtains acid leaching solution and acid leached mud, the acid leaching yield 99.03% that leaches Zn, iron 93.11%, indium 92.86%.
4, adopt in the zinc oxide acid leaching solution that obtains and heavy indium, zinc oxide dosage is 13.75% of a calcining weight, heavy indium endpoint pH 4.5, and heavy indium rate 99.47% is crossed and is filtered liquid behind heavy indium slag and the heavy indium.
After liquid mixes behind neutral leach liquor that 5, will obtain and the heavy indium, add in the autoclave and carry out the high pressure deironing, aerating oxygen; 200 ℃ of deironing temperature; Under the oxygen partial pressure 0.2MPa, 4 hours deironing time, form hematite precipitation after making the oxidation of divalent in the solution; Filtration obtains liquid and rhombohedral iron ore slag after the deironing, deironing rate 98.29%.The rhombohedral iron ore slag contains Fe61.84%, Zn1.45%, S1.98%.
6, with said rhombohedral iron ore scum with 0.5mol/L HCl agitator treating 30min; 60 ℃ of temperature; The rhombohedral iron ore that the pickling after-filtration obtains is in the retort furnace roasting, 800 ℃ of maturing temperatures, roasting time 30min; Obtain containing the brown iron oxide that meets the requirement of the industrial red stone II of HC/T2574-94 type of red stone 97.65%, productive rate 89.8%.In the washings lime with the back qualified discharging.
7, liquid after the said deironing is adopted the neutralization of fluidized bed roasting flue dust, in terminal point pH5.4, neutralizer purifies the back electrodeposition and obtains metallic zinc, in the secondary zinc oxide that after reduction volatilization, produces with slag as the neutralizing agent of the heavy indium of pickling liquor.
Embodiment 2
A kind of method of from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone may further comprise the 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, feed 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) they are 5:1, the neutral terminal point pH 5.4 that leaches; Neutral extraction time 30 min; Filtration obtain neutral leach liquor with in soak slag, neutral leaching yield Zn75.9%, the Fe53.3% of leaching.
3, carry out the acidity leaching with soaking slag in said, acid initial acidity 160g/L, 95 ℃ of the extraction temperatures of leaching; The acid terminal point acidity 10g/L that leaches, extraction time 4 hours filters and obtains acid leaching solution and acid leached mud; The acid leaching yield Zn99.0% that leaches, Fe91.8%, In90.7%.
4, adopt in the zinc oxide acid leaching solution that obtains and heavy indium, the terminal point pH4.0 of heavy indium crosses liquid behind heavy indium slag and the heavy indium, the heavy indium rate 98.6% of filtering.
After liquid mixes behind neutral leach liquor that 5, will obtain and the heavy indium, add autoclave, aerating oxygen; At 190 ℃; Keep oxygen partial pressure 0.3MPa, 3 hours deironing time, form hematite precipitation after making the oxidation of divalent in the solution; Filtration obtains liquid and rhombohedral iron ore slag after the deironing, deironing rate 97.79%.The rhombohedral iron ore slag contains Fe61.77%, Zn1.52%, S1.82%.
6, gained rhombohedral iron ore slag is with 1mol/L HCl stirring and pickling 60min; 80 ℃ of temperature; The rhombohedral iron ore that the pickling after-filtration obtains obtains containing red stone 98.05% and meets the brown iron oxide that the industrial red stone II of HC/T2574-94 type requires, productive rate 79.3% in 700 ℃ of roasting temperature 80min.
7, liquid adopts the neutralization of fluidized bed roasting flue dust after the gained deironing, in terminal point pH5.4, neutralizer purifies the back electrodeposition and obtains metallic zinc, in the secondary zinc oxide that after reduction volatilization, produces with slag as the neutralizing agent of the heavy indium of pickling liquor.
Embodiment 3
A kind of method of from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone may further comprise the steps:
1, will contain Zn53.2%, Fe18.98%, the high ferro zinc baking sand of In0.093% contact reduction with CO in rotary kiln, feed 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 with in soak slag, the neutral leaching yield 69.38% that leaches Zn, iron 55.8%.
3, carry out the acidity leaching with soaking slag in said, acid initial acidity 200g/L, 95 ℃ of the extraction temperatures of leaching; The acid terminal point acidity 50g/L that leaches, extraction time 2 hours filters and obtains acid leaching solution and acid leached mud; The acid leaching yield Zn99.7% that leaches, Fe95.8%, In92.3%.
4, adopt in the zinc oxide acid leaching solution that obtains and heavy indium, the terminal point pH4.8 of heavy indium crosses liquid behind heavy indium slag and the heavy indium, the heavy indium rate 99.9% of filtering.
Liquid mixes the back and adds autoclave behind neutral leach liquor that 5, will obtain and the heavy indium; Aerating oxygen at 170 ℃, keeps oxygen partial pressure 0.4MPa; 2 hours deironing time; Form hematite precipitation after making the oxidation of divalent in the solution, filter liquid and rhombohedral iron ore slag after the 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 was with 1mol/L HCl stirring and pickling 1.5 hours; 70 ℃ of temperature; The rhombohedral iron ore that the pickling after-filtration obtains is in 850 ℃ of roasting temperatures 1 hour, and what obtain containing red stone 97.22% meets the brown iron oxide that the industrial red stone II of HC/T2574-94 type requires, productive rate 76.9%.
7, liquid adopts the neutralization of fluidized bed roasting flue dust after the gained deironing, in terminal point pH5.4, neutralizer purifies the back electrodeposition and obtains metallic zinc, in the secondary zinc oxide that after reduction volatilization, produces with slag as the neutralizing agent of the heavy indium of pickling liquor.
Embodiment 4
A kind of method of from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone may further comprise the steps:
1, will contain Zn51.7%, Fe21.02%, the high ferro zinc baking sand of In0.096% contact reduction with CO in rotary kiln, feed 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 with in soak slag, the neutral leaching yield 84.64% that leaches Zn, iron 49.83%.
3, carry out the acidity leaching with soaking slag in said, acid initial acidity 180g/L, 80 ℃ of the extraction temperatures of leaching; The acid terminal point acidity 28g/L that leaches, extraction time 4 hours filters and obtains acid leaching solution and acid leached mud; The acid leaching yield Zn99.1% that leaches, Fe94.4%, In91.6%.
4, adopt in the zinc oxide acid leaching solution that obtains and heavy indium, the terminal point pH4.6 of heavy indium crosses liquid behind heavy indium slag and the heavy indium, the heavy indium rate 99.5% of filtering.
Liquid mixes the back and adds autoclave behind neutral leach liquor that 5, will obtain and the heavy indium; Aerating oxygen at 160 ℃, keeps oxygen partial pressure 0.4MPa; 4 hours deironing time; Form hematite precipitation after making the oxidation of divalent in the solution, filter liquid and rhombohedral iron ore slag after the 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 was with 1mol/L HCl stirring and pickling 1.5 hours; 30 ℃ of temperature; The rhombohedral iron ore that the pickling after-filtration obtains is in 850 ℃ of roasting temperatures 1 hour, and what obtain containing red stone 96.05% meets the brown iron oxide that the industrial red stone II of HC/T2574-94 type requires, productive rate 75.8%.
7, liquid adopts the neutralization of fluidized bed roasting flue dust after the gained deironing, in terminal point pH5.4, neutralizer purifies the back electrodeposition and obtains metallic zinc, in the secondary zinc oxide that after reduction volatilization, produces with slag as the neutralizing agent of the heavy indium of pickling liquor.
Claims (2)
1. method of from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone is characterized in that this method may further comprise the steps:
1.1 will contain 46～54% zinc, the high ferro 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 pH 5.4 that leaches, filtration obtain neutral leach liquor and in soak slag,
1.3 carry out acidity and leach with soaking slag in said, acidly leach initial acidity 160～200g/L, 80～95 ℃ of extraction temperatures, the acid terminal point acidity 10～50g/L that leaches, extraction time 2～4 hours is crossed and is filtered acid leaching solution and acid leached mud,
1.4 the acid leaching solution that obtains is adopted in the zinc oxide and heavy indium, and terminal point pH4～4.8 of heavy indium are crossed and are filtered liquid behind heavy indium slag and the heavy indium,
1.5 liquid mixes the back and adds autoclave behind neutral leach liquor that will obtain and the heavy indium, aerating oxygen is at 160～200 ℃; Keep oxygen partial pressure 0.2～0.4MPa, 2～4 hours deironing time, form hematite precipitation after making the oxidation of divalent in the solution; Filtration obtains liquid and rhombohedral iron ore slag after the 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; The rhombohedral iron ore that the pickling after-filtration obtains obtains meeting the brown iron oxide that the industrial red stone II of HC/T2574-94 type requires in 600～900 ℃ of roasting temperatures 0.5～1 hour
1.7 liquid adopts the neutralization of fluidized bed roasting flue dust after the gained deironing, in terminal point pH5.4, neutralizer purifies the back electrodeposition and obtains metallic zinc, in the secondary zinc oxide that after reduction volatilization, produces with slag as the neutralizing agent of the heavy indium of pickling liquor.
2. the method for from contain high ferro indium zinc baking sand, extracting indium zinc and preparing red stone according to claim 1 is characterized in that said reduced calcine is at N
2Protection cooling down.
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| 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 |
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| CN103276197A (en) * | 2013-05-17 | 2013-09-04 | 中南大学 | Method for performing flash reducing and roasting on zinc calcine |
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| 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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| CN115109920B (en) * | 2022-06-20 | 2023-09-22 | 云锡文山锌铟冶炼有限公司 | Method for reducing zinc and sulfur in hematite by zinc hydrometallurgy system |
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