CN103952562A - Comprehensive utilization method of iron vitriol slag - Google Patents
Comprehensive utilization method of iron vitriol slag Download PDFInfo
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- CN103952562A CN103952562A CN201410219456.7A CN201410219456A CN103952562A CN 103952562 A CN103952562 A CN 103952562A CN 201410219456 A CN201410219456 A CN 201410219456A CN 103952562 A CN103952562 A CN 103952562A
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- iron
- zinc
- vitriol slag
- slag
- iron vitriol
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
A method for comprehensively utilizing iron vitriol slag is characterized in that in zinc hydrometallurgy, a method for mixing and leaching a hot acid leaching liquid, zinc concentrate and iron vitriol slag is adopted, acid produced by hematite through hydrolysis of iron in the hot acid leaching liquid and iron in the iron vitriol slag and residual acid in the hot acid leaching liquid are utilized to leach zinc concentrate, and multiple targets of zinc concentrate leaching, iron removal, iron vitriol slag treatment, comprehensive recovery of valuable metals and the like are achieved. Crushing and grinding zinc concentrate and iron vitriol slag, adding the crushed and ground zinc concentrate and a first-stage hot acid leaching solution into a pressure reaction kettle, flashing and thickening the leached ore pulp, returning the supernatant to neutral leaching, washing the underflow, and performing filter pressing to obtain goethite slag. The invention can achieve zinc recovery rate: 83 percent; recovery rate of scattered metals: > 75%; and iron recovery rate: 65 percent; grade of iron ore concentrate: over 55 percent, realizes the comprehensive recycling of the jarosite slag and has great economic and social significance.
Description
Technical field
The invention belongs to technical field of wet metallurgy, relate to iron vitriol slag method of comprehensive utilization in a kind of zinc wet smelting process.
Background technology
China's zinc output 85% by zinc hydrometallurgy output, in zinc hydrometallurgy, have 45% output to produce by heat acid leaching-ferro-alum deironing.The siderotil quantity of slag of heat acid leaching-ferro-alum deferrization process output is large, it is large to pollute, and the whole nation is stored up the siderotil quantity of slag and exceeded 3,000 ten thousand tons and have pendingly, and annual by the speed increment with 1,000,000 tons, and environment is produced to huge potentially contaminated; Metal loss is large simultaneously, if iron vitriol slag calculates containing zinc 5% by average, accumulates zinc amount of metal and exceedes 1,500,000 tons, and utility value is very high.Based on above 2 points, to iron vitriol slag further investigation, turn waste into wealth, be significant.
At present, the processing of iron vitriol slag mainly concentrates on innoxious fixing processing and reclaims valuable metal two aspects.The innoxious technique for fixing of iron vitriol slag can be divided into high-temperature sintering process, reducing roasting-magnetic method, roasting-lixiviation process and solvent extraction method etc., and the iron resources in iron vitriol slag is respectively with silicate, wustite or Fe
2o
3obtain increment utilization in fields such as ironmaking, devitrified glass, stupalith, pigment or building materials etc. form, heavy metal element obtains efficient recovery or solidification treatment.But because operation cost is high, these techniques are not all applied.Having realized industrialized iron vitriol slag treatment process is mainly fuming process, as Weng Shan smeltery of Korea S adopts the valuable metal in two sections of recyclable slags of Ausmelt stove, but this technique fixed investment and running cost are all higher, and also can cause atmospheric pollution in vaporization at high temperature process.Therefore, how to process cost-effectively the huge zinc hydrometallurgy iron vitriol slag of quantity, remain the important environmental protection subject that current colored metallurgical industrial faces.
Summary of the invention
The object of this invention is to provide a kind of method of iron vitriol slag comprehensive utilization, recycle the valuable metal in iron vitriol slag, make iron vitriol slag become rhombohedral iron ore simultaneously, realize triple targets of Zinc Concentrate Leaching, leach liquor deironing and the processing of ferrovanadium slag.
Object of the present invention is achieved through the following technical solutions.
A method for iron vitriol slag comprehensive utilization, comprises the following steps:
(1) pressure leaching: after zinc ore concentrate and iron vitriol slag fragmentation, and the hot acid leach liquor of zinc hydrometallurgy system is mixed with ore pulp, joins in autoclave, passes into air or oxygen, realizes oxygen and presses to mix and leach;
(2) liquid-solid separation: after having leached, ore pulp is after flash distillation, dense processing, and the neutrality that supernatant liquor is back to zinc hydrometallurgy system leaches operation;
(3) dense washing: the underflow after dense carries out the dense washing of CCD adverse current, the supernatant liquor after washing is back to step (2);
(4) press filtration: by the underflow press filtration after dense washing, filtrate is back to step (3), and filter cake is stored up, and obtains rhombohedral iron ore slag.
In step (1), zinc ore concentrate, iron vitriol slag and hot acid leach liquor after fragmentation are mixed with ore pulp, add in autoclave, iron vitriol slag can be one or more in sodium alum, arcanite and ammonium alum, adaptability to raw material is strong, the type of iron vitriol slag is not limit to applied range.The initial ore pulp liquid-solid ratio of pressure leaching 3～15:1,130～220 DEG C of extraction temperatures, extraction time 1～8h, oxygen partial pressure 2～10atm, zinc ore concentrate accounts for zinc ore concentrate and iron vitriol slag solid mixture mass ratio is 0～80%.The leaching yield > 83% of zinc with this understanding, dissipated metal rate of recovery > 75%, the deposition rate > 80% of iron, iron recovery > 65%.The following reaction of main generation in leaching process:
Iron vitriol slag becomes rhombohedral iron ore:
2AFe
3(SO
4)
2(OH)
6=3Fe
2o
3+ A
2sO
4+ 3H
2sO
4+ 3H
2(A represents Na to O, K, NH
4)
Zinc ore concentrate oxygen is pressed and is leached:
ZnS+H
2SO
4+O
2＝ZnSO
4+S+H
2O
Fe in hot acid leach liquor
3+become rhombohedral iron ore:
2Fe
3++3H
2O＝Fe
2O
3+6H
+
Fe in iron vitriol slag and hot acid leach liquor
3+while becoming rhombohedral iron ore, all have sour output.And the leaching process of zinc ore concentrate is the sour process of consumption, control suitable reaction conditions, can realize Zinc Concentrate Leaching, leach liquor deironing and iron vitriol slag and process triple targets.
The leaching of zinc ore concentrate needs higher acidity, and why rhombohedral iron ore can be based on Fe under high temperature (200 DEG C) condition by stable existence
2o
3it is negative that acid-soluble balance pH value becomes.In the time of 25 DEG C by the Fe of solution
3+content drops to 10
-6, Fe
2o
3the balance pH=1.76 dissolving, is equivalent to sulfuric acid 2～3g/L.And temperature is while being elevated to 200 DEG C, balance pH but drops to 0.42, is equivalent to sulfuric acid 150g/L, and acidity is higher, and this illustrates that high acid medium also can make iron with Fe
2o
3precipitation exists, and Zn
2+still be retained in solution.This is that zinc ore concentrate and iron vitriol slag can mix the key point leaching.
In step (2), Zn after pressure leaching
2+enter solution, Fe
3+form with rhombohedral iron ore enters in slag.Ore pulp, through dense sedimentation, contains Zn
2+be back to the neutral operation that leaches with the supernatant liquor of residual acid, utilize residual acid wherein to carry out Leaching Zinc concentrate.
In step (3), the underflow of step (2) contains the Zn being mingled with
2+with residual acid, after the dense washing of multi-stage countercurrent, underflow press filtration, supernatant liquor is back to step (2).
In step (4), the filter cake that press filtration obtains is rhombohedral iron ore slag, containing Fe
2o
3amount > 55%.
The present invention utilized dexterously rhombohedral iron ore under hot conditions can be in the high acid medium principle of stable existence, a kind of method of iron vitriol slag comprehensive utilization is provided, the hot acid leach liquor pressurization of iron vitriol slag, zinc ore concentrate and zinc hydrometallurgy system is mixed and leached, both realized the recycling of iron vitriol slag, make its resource utilization, realized again the deironing of hot acid leach liquor and the leaching of zinc ore concentrate.Particularly, in pressure leaching process, the zinc of carrying secretly in iron vitriol slag is reclaimed, and the iron in iron vitriol slag and hot acid leach liquor, with the form output of rhombohedral iron ore, can be used as the raw material of ironmaking, makes its resource utilization or stores up; Utilize in hot acid leach liquor molten iron solution in iron and iron vitriol slag to generate the acid of rhombohedral iron ore output simultaneously, and the residual Ore Leaching zinc ore concentrate that has of hot acid leach liquor itself.The method adaptability to raw material is strong, applied widely, compares with other techniques, takes full advantage of Fe
3+the acid that hydrolysis produces, has reduced sulfuric acid consumption, and zinc leaching rate is high, has reduced tailings quantity discharged.The method turns waste into wealth, consumption reduction reduces discharging, and has both had significant economic benefit, has again great social benefit.
Brief description of the drawings
Accompanying drawing is the process flow sheet that uses iron vitriol slag method of comprehensive utilization of the present invention in zinc wet smelting process.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described.
Accompanying drawing is the process flow sheet that uses iron vitriol slag method of comprehensive utilization of the present invention in zinc wet smelting process, and wherein dotted line frame inside is divided into the process flow sheet of iron vitriol slag method of comprehensive utilization of the present invention, and other parts are the traditional technology of zinc hydrometallurgy.
A method for iron vitriol slag comprehensive utilization, comprises the following steps:
(1) pressure leaching: after zinc ore concentrate and iron vitriol slag fragmentation, and the hot acid leach liquor of zinc hydrometallurgy system is mixed with ore pulp, joins in autoclave, passes into air or oxygen, realizes oxygen and presses to mix and leach.The initial ore pulp liquid-solid ratio of pressure leaching 3～15:1,130～220 DEG C of extraction temperatures, extraction time 1～8h, oxygen partial pressure 2～10atm, zinc ore concentrate accounts for solid mixture ratio 0～80%.The leaching yield > 83% of zinc with this understanding, dissipated metal rate of recovery > 75%, the deposition rate > 80% of iron, iron recovery > 65%.
(2) liquid-solid separation: after having leached, ore pulp is after flash distillation, dense processing, and the neutrality that supernatant liquor is back to zinc hydrometallurgy system leaches operation.
(3) dense washing: the underflow after dense carries out the dense washing of CCD adverse current, the supernatant liquor after washing is back to step (2).
(4) press filtration: by the underflow press filtration after dense washing, filtrate is back to step (3), and filter cake is stored up, and obtains rhombohedral iron ore slag.
The method leaches by the mixing of zinc ore concentrate, iron vitriol slag and hot acid leach liquor, has both recycled the valuable metal in iron vitriol slag, makes iron vitriol slag become rhombohedral iron ore simultaneously, realizes triple objects of Zinc Concentrate Leaching, leach liquor deironing and the processing of ferrovanadium slag.
The iron vitriol slag of the method processing can be one or more in sodium alum, arcanite and ammonium alum, adaptability to raw material is strong, type to iron vitriol slag is not limit, applied range, compare with other techniques, both realize the recycling of iron vitriol slag, made its resource utilization, realized again the deironing of hot acid leach liquor and the leaching of zinc ore concentrate.This invention takes full advantage of Fe
3+the acid that hydrolysis produces, has reduced sulfuric acid consumption, and zinc leaching rate is high, has reduced tailings quantity discharged.
Embodiment 1
Get the zinc ore concentrate (Zn45.67% after fragmentation, Fe11.7%, S30.73%) 33.3g (dry meter), iron vitriol dreg of yellow sodium (Zn3.75%, Fe27.26%, S13.26%) 66.6g (dry meter), hot acid leach liquor (Zn113.47g/L, Fe8g/L, H
2sO
47.07g/L) 900ml, is mixed, and is mixed with ore pulp and adds in autoclave.Pass into oxygen press 6atm, 200 DEG C of temperature of reaction, reaction time 4h.The leaching yield of having reacted rear Zn is 98.11%, and leach liquor is containing Zn127.37g/L, Fe1.1g/L, H
2sO
415.64g/L.
Embodiment 2
Get zinc ore concentrate (Zn45.67%, Fe11.7%, the S30.73%) 50g (dry meter) after fragmentation, iron vitriol dreg of yellow sodium (Zn3.75%, Fe27.26%, S13.26%) 50g (dry meter), hot acid leach liquor (Zn113.47g/L, Fe8g/L, H
2sO
47.07g/L) 500ml, is mixed, and is mixed with ore pulp and adds in autoclave.Pass into oxygen press 6atm, 180 DEG C of temperature of reaction, reaction time 2h.The leaching yield of having reacted rear Zn is 85.66%, and leach liquor is containing Zn137.11g/L, Fe1.62g/L, H
2sO
422.4g/L.
Embodiment 3
Get zinc ore concentrate (Zn45.67%, Fe11.7%, the S30.73%) 25g (dry meter) after fragmentation, Jarosite Residues (Zn3.18%, Fe25.68%, S11.26%) 75g (dry meter), hot acid leach liquor (Zn113.47g/L, Fe8g/L, H
2sO
47.07g/L) 900ml, is mixed, and is mixed with ore pulp and adds in autoclave.Pass into oxygen press 6atm, 180 DEG C of temperature of reaction, reaction time 4h.The leaching yield of having reacted rear Zn is 86.31%, and leach liquor is containing Zn131.75g/L, Fe1.54g/L, H
2sO
422.82g/L.
Embodiment 4
Get zinc ore concentrate (Zn45.67%, Fe11.7%, the S30.73%) 25g (dry meter) after fragmentation, Jarosite Residues (Zn3.18%, Fe25.68%, S11.26%) 75g (dry meter), hot acid leach liquor (Zn113.47g/L, Fe8g/L, H
2sO
47.07g/L) 900ml, is mixed, and is mixed with ore pulp and adds in autoclave.Pass into oxygen press 3atm, 200 DEG C of temperature of reaction, reaction time 2h.The leaching yield of having reacted rear Zn is 85.69%, and leach liquor is containing Zn132.17g/L, Fe1.68g/L, H
2sO
423.24g/L.
Claims (5)
1. a method for iron vitriol slag comprehensive utilization, is characterized in that, comprises the following steps:
(1) pressure leaching: after zinc ore concentrate and iron vitriol slag fragmentation, and the hot acid leach liquor of zinc hydrometallurgy system is mixed with ore pulp, joins in autoclave, passes into air or oxygen, realizes oxygen and presses to mix and leach;
(2) liquid-solid separation: after having leached, ore pulp is after flash distillation, dense processing, and the neutrality that supernatant liquor is back to zinc hydrometallurgy system leaches operation;
(3) dense washing: the underflow after dense carries out the dense washing of CCD adverse current, the supernatant liquor after washing is back to step (2);
(4) press filtration: by the underflow press filtration after dense washing, filtrate is back to step (3), and filter cake is stored up, and obtains rhombohedral iron ore slag.
2. the method for claim 1, is characterized in that, in step (1), pulp slurry is admittedly than 3～15:1.
3. the method for claim 1, is characterized in that, oxygen described in step (1) presses mixing extract technology condition to be: 130～220 DEG C of extraction temperatures, extraction time 1～8h, oxygen partial pressure 2～10atm.
4. the method for claim 1, is characterized in that, it is 0～80% with iron vitriol slag mixture quality ratio that the middle zinc ore concentrate of step (1) accounts for zinc ore concentrate.
5. the method for claim 1, is characterized in that, in step (1), iron vitriol slag is one or more in sodium alum, arcanite and ammonium alum.
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|---|---|---|---|
| CN201410219456.7A CN103952562A (en) | 2014-05-22 | 2014-05-22 | Comprehensive utilization method of iron vitriol slag |
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|---|---|---|---|
| CN201410219456.7A CN103952562A (en) | 2014-05-22 | 2014-05-22 | Comprehensive utilization method of iron vitriol slag |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106244817A (en) * | 2016-08-31 | 2016-12-21 | 汉中锌业有限责任公司 | A kind of technique of resource pretreatment zinc abstraction low stain jarosite process iron vitriol slag |
| 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 |
| CN109607622A (en) * | 2019-01-03 | 2019-04-12 | 昆明理工大学 | A method of iron oxide red product is prepared using the heavy scum of zinc hydrometallurgy hematite process |
| CN110255770A (en) * | 2019-07-03 | 2019-09-20 | 昆明理工大学 | A kind of method that Jarosite Residues cooperate with arsenic in calcium carbide Slag treatment nonferrous smelting waste acid |
| CN110872650A (en) * | 2018-08-31 | 2020-03-10 | 呼伦贝尔驰宏矿业有限公司 | Leaching method of zinc concentrate |
| CN111041210A (en) * | 2019-12-10 | 2020-04-21 | 赤峰中色锌业有限公司 | Comprehensive recovery and harmless treatment method for zinc hydrometallurgy jarosite slag and high leaching slag |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106244817A (en) * | 2016-08-31 | 2016-12-21 | 汉中锌业有限责任公司 | A kind of technique of resource pretreatment zinc abstraction low stain jarosite process iron vitriol slag |
| 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 |
| CN110872650A (en) * | 2018-08-31 | 2020-03-10 | 呼伦贝尔驰宏矿业有限公司 | Leaching method of zinc concentrate |
| CN109607622A (en) * | 2019-01-03 | 2019-04-12 | 昆明理工大学 | A method of iron oxide red product is prepared using the heavy scum of zinc hydrometallurgy hematite process |
| CN110255770A (en) * | 2019-07-03 | 2019-09-20 | 昆明理工大学 | A kind of method that Jarosite Residues cooperate with arsenic in calcium carbide Slag treatment nonferrous smelting waste acid |
| CN110255770B (en) * | 2019-07-03 | 2022-05-27 | 昆明理工大学 | Method for treating arsenic in nonferrous smelting waste acid by using jarosite slag and carbide slag |
| CN111041210A (en) * | 2019-12-10 | 2020-04-21 | 赤峰中色锌业有限公司 | Comprehensive recovery and harmless treatment method for zinc hydrometallurgy jarosite slag and high leaching slag |
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