CN104561564A - Method for recovering copper, silver and iron from wet zinc smelting rotary kiln slag - Google Patents
Method for recovering copper, silver and iron from wet zinc smelting rotary kiln slag Download PDFInfo
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- CN104561564A CN104561564A CN201410833981.8A CN201410833981A CN104561564A CN 104561564 A CN104561564 A CN 104561564A CN 201410833981 A CN201410833981 A CN 201410833981A CN 104561564 A CN104561564 A CN 104561564A
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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
Abstract
The invention discloses a method for recovering copper, silver and iron from wet zinc smelting rotary kiln slag. The method comprises the following steps: 1, performing ore grinding and magnetic separation on the wet zinc smelting rotary kiln slag to obtain magnetic ore powder; 2, performing ore mixing: mixing the magnetic ore power and pyrite powder with sulfur and iron content of more than 90 percent to obtain mixed ore powder; 3, performing oxidative desulfurization roasting: performing roasting desulfurization treatment to obtain sulfur dioxide and desulfurized ore powder; 4, performing chlorination roasting: mixing a chlorination agent, an adhesive, water and the desulfurized ore powder to obtain pellets, and performing chlorination roasting treatment to obtain copper chloride and silver chloride flue gas and roasted pellets. According to the method, the magnetic ore powder in the wet zinc smelting rotary kiln slag is magnetically separated and recovered, so that copper and silver densely symbiotic with the magnetic ore powder are recovered, and meanwhile, the pellets with iron content of more than 50 percent are obtained.
Description
Technical field
The invention belongs to metal recovery and utilize technical field, be specifically related to a kind of method reclaiming copper, silver and iron from zinc hydrometallurgy revolution kiln slag.
Background technology
In Zinc Hydrometallurgy Process, valuable metal major part beyond dezincification in zinc concentrate is enriched in leached mud, after adopting rotary kiln vaporization at high temperature to reclaim wherein residual zinc, remaining revolution kiln slag also contains the valuable component such as copper, silver, simultaneously containing the element such as iron and sulphur.Rotary kiln vaporization at high temperature zinc carries out under interpolation sulfur-bearing coal makes the condition of reducing agent and fuel, so iron part forms tri-iron tetroxide and the magnetic iron ore of magnetic, and the sulphur in sulphur coal enters in magnetic iron ore.Thus, the copper in From Zinc Hydrometallurgy Residue and silver also major part change into copper sulfide and silver sulfide, with magnetic iron ore, magnetic iron ore symbiosis.Because this artificial mineral structure composition is extremely complicated, simple ore dressing is difficult to realize copper, silver is separated with iron content containing sulfur minerals, causes to extract valuable metal cost-effectively; In addition, mineral resources supply is becoming tight contradiction day, and the focus of domestic coloured industry competition to be occupied transferring to and resource comprehensive utilization utilizes in technology voluntary.Therefore, the hot issue of ore dressing field research has been become from leaching comprehensively recovering valuable metal cadmia.
It is recover silver that the object of cadmia is leached in floatation process process, and the silver in cadmia mainly exists with sulfide and morphon, and silver is distributed in-200 orders in flotation size fraction ranges, can adopt direct flotation method.Floatation technological process is short, and producing cost is low, and weak point is that the existence of zinc ion causes floatation indicators to worsen, and the character of the rate of recovery of silver and leached mud and the feature of manufacturer have substantial connection, and as silver is seriously wrapped up, the rate of recovery declines to a great extent.
Except the copper adopted in floatation extraction zinc leaching residue and silver, Recovering Copper silver mode also has wet-leaching enrichment and fire enrich.Under weak oxide condition, silver can be dissolved in containing Fe
3+with in the diluted acid of thiocarbamide, form soluble cation complex compound, thiocarbamide extract technology, silver recovery rate is high, but thiocarbamide self is expensive, not as cyanide is stablized, and copper ion can be combined with thiocarbamide and forms complex compound, cause the consumption of thiocarbamide large, high cost, thus the suitability for industrialized production limiting this method.Villaumite method is under acid condition and oxidant exist, and makes silver sulfide oxidation in leached mud, silver ion enter solution and with the chlorion complexing in solution.But this reaction condition requires that the acidity of medium is strong, and villaumite concentration is high, and reaction temperature is high, can severe corrosion equipment.
The emphasis of rotary kiln evaporation technique is the recovery of lead, zinc and indium, and the disadvantage of this technique is that kiln wall bonding causes kiln short for age, and refractory consumption rate is large, and energy consumption is high.The essence of fuming furnace process zinc leaching residue technique or volatilization process, principle is substantially identical with rotary kiln evaporation technique, and be carry out in the liquid phase unlike fuming process, the valuable metal of technique institute output reclaims with oxide form, is mainly used in liquid slag.
The zinc leaching residue of the cupric silver that zinc abstraction factory all wants output a large amount of every year, this leached mud is after rotary kiln evaporation zinc, and copper and silver fail effectively to be reclaimed, and not only waste ample resources, also have certain pollution to environment, and affect the economic benefit of enterprise.Along with economic development is to the growth of non-ferrous metal demand, enterprise is impelled to excavate valuable metal potentiality such as copper, silver in zinc leaching residue further, for synthetical recovery metal provides driving force.On the other hand, valuable metal is worth and significantly improves, and ensure that the economy of valuable metal synthetical recovery in zinc leaching residue.If adopt a kind of reasonably technique, make the valuable component synthetical recovery such as valuable metal copper, silver in zinc leaching residue, by the good economic benefit of generation and environmental benefit.
Summary of the invention
In order to overcome the defect that above-mentioned prior art exists, the object of the present invention is to provide a kind of method reclaiming copper, silver and iron from zinc hydrometallurgy revolution kiln slag, the present invention reclaims the magnetic mineral fine in zinc hydrometallurgy revolution kiln slag by magnetic separation, thus reclaim copper and the silver of the fine and close symbiosis with magnetic mineral fine, obtain simultaneously iron content higher than 50% pellet.
For achieving the above object, the present invention adopts following technical scheme:
From zinc hydrometallurgy revolution kiln slag, reclaim a method for copper, silver and iron, comprise the following steps:
1) magnetic separation: zinc hydrometallurgy is turned round kiln slag and carry out ore grinding process, then carries out magnetic separation by the zinc hydrometallurgy revolution kiln slag after ore grinding process, obtains magnetic mineral fine;
2) join ore deposit: by step 1) in the magnetic mineral fine that obtains mix with troilite powder, obtain mixed mineral powder;
3) desulfurization with roasting technique: to step 2) mixed mineral powder that obtains carries out desulfurization with roasting technique process, obtains sulfur dioxide and desulfurization breeze;
4) chloridising roasting: ((the desulfurization breeze obtained in 0.5 ~ 1) ﹕ (8 ~ 11) ﹕ 100 are by chlorinating agent, binding agent, water and step 3) makes pelletizing after mixing to 5 ~ 10) ﹕ in mass ratio, then pelletizing is carried out chloridising roasting process, obtain silver chlorate flue gas and copper chloride flue gas and pellet.
Further, in the zinc hydrometallurgy revolution kiln slag after described ore grinding process, the rotary kiln slag mass percentage of-200 order grades is greater than 60%.
Further, step 1) described in magnetic separation be carry out under magnetic field intensity is the condition of 2000 ~ 6000Oe.
Further, step 2) described in troilite powder in the gross mass mark of sulfur-bearing and iron be greater than 90%; In mixed mineral powder, the mass fraction of sulfur-bearing is greater than 25%.
Further, step 3) in the temperature of desulfurization with roasting technique be 850 ~ 950 DEG C.
Further, step 4) described in chlorinating agent be one in calcium chloride, sodium chloride or ammonium chloride.
Further, step 4) described in binding agent be one in bentonite or pellet binder.
Further, step 4) described in pelletizing diameter be 8 ~ 12mm.
Further, step 4) described in chloridising roasting temperature be 1000 ~ 1100 DEG C.
Further, step 4) described in the chloridising roasting time be 90 ~ 120min.
Compared with prior art, the present invention has following useful technique effect:
Containing the iron of about 25% in zinc hydrometallurgy revolution kiln slag, in rotary kiln baking process, iron may be reduced into the magnetic magnetic iron ore of tool and magnetic iron oxide, and in the process of rotary kiln reduction roasting dezincify, copper and silver are sulphophile elements, sulfuration easily and in the coal of leached mud and interpolation is closed and is formed sulfide, magnetic iron ore magnetic with tool, magnetic iron ore symbiosis and obtain enrichment, the present invention adopts the magnetic separator of modest magnetic field can reclaim magnetic iron ore and the magnetic iron ore of magnetic, also copper and silver have just been reclaimed simultaneously, the magnetic mineral fine sulfur-bearing grade of the cupric silver of magnetic concentration is less than 18%, when directly entering boiling roaster, because of shortage of heat, be difficult to the thermal balance maintaining boiling furnace combustion, with other mode desulfurization with roasting technique, the flue gas obtained is low containing sulfur dioxide concentration, Sulphuric acid difficulty, so, the present invention adds the high troilite powder of sulfur-bearing and carries out joining ore deposit, with the sulfur dioxide concentration requirement of the thermal balance requirement and Sulphuric acid flue gas that meet fluidized bed roasting, chloridising roasting is carried out after desulfurization breeze pelletizing, the volatility of copper and silver is greater than 90%, significantly improve the rate of recovery of valuable metal, after recovery copper and silver, also obtain iron content higher than 50% pellet.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiments of the present invention are described in further detail:
See Fig. 1, a kind of method reclaiming copper, silver and iron from zinc hydrometallurgy revolution kiln slag, comprises the following steps:
1) magnetic separation: in zinc hydrometallurgy revolution kiln slag, the mass percentage of copper is 0.5% ~ 1.0%, and the mass percentage of silver is 100g/t ~ 300g/t; The mass percentage of iron is 20% ~ 30%, zinc hydrometallurgy is turned round kiln slag and carry out ore grinding process, the rotary kiln slag mass percentage making the zinc hydrometallurgy after ore grinding process turn round-200 order grades in kiln slag is greater than 60%, then the zinc hydrometallurgy revolution kiln slag after ore grinding process is placed in magnetic separator, be carry out magnetic separation under the condition of 2000 ~ 6000Oe in magnetic field intensity, obtain magnetic mineral fine;
2) join ore deposit: by step 1) in the gross mass mark of the magnetic mineral fine that obtains and sulfur-bearing and the iron troilite powder that is greater than 90% mix, the mass fraction obtaining sulfur-bearing is greater than the mixed mineral powder of 25%;
3) desulfurization with roasting technique: to step 2) mixed mineral powder that obtains carries out desulfurization with roasting technique process at the temperature of 850 ~ 950 DEG C, obtains sulfur dioxide and desulfurization breeze;
4) chloridising roasting: ((the desulfurization breeze obtained in 0.5 ~ 1) ﹕ (8 ~ 11) ﹕ 100 are by chlorinating agent, binding agent, water and step 3) makes the pelletizing that diameter is 8 ~ 12mm after mixing to 5 ~ 10) ﹕ in mass ratio, wherein chlorinating agent is the one in calcium chloride, sodium chloride or ammonium chloride, binding agent is the one in bentonite or pellet binder, then pelletizing is placed in rotary kiln, chloridising roasting 90 ~ 120min at the temperature of 1000 ~ 1100 DEG C, namely obtains silver chlorate flue gas and copper chloride flue gas and pellet.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
In the present embodiment in zinc hydrometallurgy revolution kiln slag, in mass fraction, cupric 0.95%, argentiferous 132.48g/t, iron content 23.76%, sulfur-bearing 9.53%; 1) this zinc hydrometallurgy revolution kiln slag is carried out ore grinding process, the rotary kiln slag mass percentage making the zinc hydrometallurgy after ore grinding process turn round-200 order grades in kiln slag is about 80%, then be carry out magnetic separation under the condition of 4000Oe in magnetic field intensity, obtain magnetic separation breeze; 2) obtained magnetic separation breeze is allocated into the high-grade troilite of sulfur-bearing and iron total more than 90% by the mass ratio of 1 ﹕ 1, obtain the mixed mineral powder that sulfur mass fraction is 35%; 3) mixed mineral powder is carried out oxidizing roasting desulfurization in the fluidized bed furnace of sintering temperature 850 DEG C, collect flue gas (sulfur dioxide) Sulphuric acid, also obtain desulfurization breeze; 4) calcium chloride, bentonite, water and the desulfurization breeze mass ratio according to 5 ﹕ 0.5 ﹕ 8 ﹕ 100 is mixed and makes the pelletizing that diameter is 8mm, then pelletizing is placed in rotary kiln, chloridising roasting 90min at the temperature of 1000 DEG C, namely silver chlorate flue gas and copper chloride flue gas and pellet is obtained, the volatility of copper, silver is greater than 90%, the pellet ferrous grade obtained is greater than 50%, sulfur-bearing is less than 0.4%, by joining ore deposit process, the copper of magnetic separation breeze, silver, iron, sulphur are obtained for efficient recycling.
Embodiment 2
In the present embodiment in zinc hydrometallurgy revolution kiln slag, in mass fraction, containing copper 0.88%, silver-colored 116g/t, iron 25.04%, sulphur 8.90%, zinc 0.54%; 1) this zinc hydrometallurgy revolution kiln slag is carried out ore grinding process, the rotary kiln slag mass percentage making the zinc hydrometallurgy after ore grinding process turn round-200 order grades in kiln slag is about 60%, then be carry out magnetic separation under the condition of 2000Oe in magnetic field intensity, obtain the magnetic separation breeze of 35%-40%, iron content about 40% in this magnetic mineral fine, copper and silver 60% are enriched in wherein; 2) obtained magnetic separation breeze is allocated into the high-grade troilite of sulfur-bearing and iron total more than 90% by the mass ratio of 1 ﹕ 1, obtain the mixed mineral powder that sulfur mass fraction is 38%; 3) mixed mineral powder is carried out oxidizing roasting desulfurization in the fluidized bed furnace of sintering temperature 900 DEG C, collect flue gas (sulfur dioxide) Sulphuric acid, also obtain desulfurization breeze; 4) sodium chloride, bentonite, water and the desulfurization breeze mass ratio according to 10 ﹕ 1.0 ﹕ 11 ﹕ 100 is mixed and makes the pelletizing that diameter is 10mm, then pelletizing is placed in rotary kiln, chloridising roasting 100min at the temperature of 1100 DEG C, namely silver chlorate flue gas and copper chloride flue gas and pellet is obtained, the volatility of copper, silver is greater than 90%, the pellet ferrous grade obtained is greater than 58%, sulfur-bearing is less than 0.4%, by joining ore deposit process, the copper of magnetic separation breeze, silver, iron, sulphur are obtained for efficient recycling.
Embodiment 3
In the present embodiment in zinc hydrometallurgy revolution kiln slag, in mass fraction, containing copper 0.85%, silver-colored 127.3g/t, iron 24.7%, sulphur 0.92%; 1) this zinc hydrometallurgy revolution kiln slag is carried out ore grinding process, the rotary kiln slag mass percentage making the zinc hydrometallurgy after ore grinding process turn round-200 order grades in kiln slag is about 70%, then be carry out magnetic separation under the condition of 6000Oe in magnetic field intensity, obtain magnetic separation breeze; 2) obtained magnetic separation breeze is allocated into the high-grade troilite of sulfur-bearing and iron total more than 90% by the mass ratio of 1 ﹕ 1, obtain the mixed mineral powder that sulfur mass fraction is 37%; 3) mixed mineral powder is carried out oxidizing roasting desulfurization in the fluidized bed furnace of sintering temperature 950 DEG C, collect flue gas (sulfur dioxide) Sulphuric acid, also obtain desulfurization breeze; 4) ammonium chloride, pellet binder, water and the desulfurization breeze mass ratio according to 8 ﹕ 1.0 ﹕ 10 ﹕ 100 is mixed and makes the pelletizing that diameter is 12mm, then pelletizing is placed in rotary kiln, chloridising roasting 120min at the temperature of 1100 DEG C, namely silver chlorate flue gas and copper chloride flue gas and pellet is obtained, the volatility of copper, silver is greater than 90%, the pellet ferrous grade obtained is greater than 50%, sulfur-bearing is less than 0.4%, by joining ore deposit process, the copper of magnetic separation breeze, silver, iron, sulphur are obtained for efficient recycling.
Copper and silver are generally uniformly distributed among various mineral, so be difficult to be reclaimed by the method for direct ore dressing with other routines in zinc hydrometallurgy revolution kiln slag.But in the process of rotary kiln reduction roasting dezincify, copper and silver are sulphophile elements, sulfuration easily and in the coal of leached mud and interpolation is closed and is formed sulfide, with the magnetic magnetic iron ore of tool, magnetic iron ore symbiosis and obtain enrichment, adopt the magnetic separator of modest magnetic field can reclaim magnetic iron ore and the magnetic iron ore of magnetic, also just reclaim copper and silver simultaneously.
The magnetic mineral sulfur-bearing grade of the cupric silver of magnetic concentration is less than 18%, when directly entering boiling roaster, because of shortage of heat, be difficult to the thermal balance maintaining boiling furnace combustion, with other mode desulfurization with roasting technique, the flue gas obtained is low containing sulfur dioxide concentration, Sulphuric acid difficulty, so, the troilite adding sulfur-bearing high carries out joining ore deposit, obtain the compound that sulfur-bearing is greater than 25%, meet the thermal balance requirement of fluidized bed roasting and the sulfur dioxide concentration requirement of Sulphuric acid flue gas, ensure that the low-sulfur in cadmia is effectively reclaimed.Desulfurization slag iron content reaches more than 50%, creates favorable conditions, the iron in cadmia is recycled for next step chloridising roasting obtains qualified pellet.By allocating high-grade troilite into, the unserviceable iron of script and sulphur in cadmia is made all to become recyclable resource.
Fluidized bed furnace slag passes through chloridising roasting, copper and silver form chloride-sublimation, the volatility of copper and silver is greater than 90%, significantly improve the rate of recovery of valuable metal, obtaining copper silver bulk concentrate product by flue gas dust collection send smelting to reclaim copper and silver, recovery copper and silver after, also obtain iron content higher than 50% pellet.
Claims (10)
1. from zinc hydrometallurgy revolution kiln slag, reclaim a method for copper, silver and iron, it is characterized in that, comprise the following steps:
1) magnetic separation: zinc hydrometallurgy is turned round kiln slag and carry out ore grinding process, then carries out magnetic separation by the zinc hydrometallurgy revolution kiln slag after ore grinding process, obtains magnetic mineral fine;
2) join ore deposit: by step 1) in the magnetic mineral fine that obtains mix with troilite powder, obtain mixed mineral powder;
3) desulfurization with roasting technique: to step 2) mixed mineral powder that obtains carries out desulfurization with roasting technique process, obtains sulfur dioxide and desulfurization breeze;
4) chloridising roasting: ((the desulfurization breeze obtained in 0.5 ~ 1) ﹕ (8 ~ 11) ﹕ 100 are by chlorinating agent, binding agent, water and step 3) makes pelletizing after mixing to 5 ~ 10) ﹕ in mass ratio, then pelletizing is carried out chloridising roasting process, obtain silver chlorate flue gas and copper chloride flue gas and pellet.
2. a kind of method reclaiming copper, silver and iron from zinc hydrometallurgy revolution kiln slag according to claim 1, is characterized in that, in the zinc hydrometallurgy revolution kiln slag after described ore grinding process, the rotary kiln slag mass percentage of-200 order grades is greater than 60%.
3. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaim the method for copper, silver and iron, it is characterized in that, step 1) described in magnetic separation be carry out under magnetic field intensity is the condition of 2000 ~ 6000Oe.
4. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaim the method for copper, silver and iron, it is characterized in that, step 2) described in troilite powder in the gross mass mark of sulfur-bearing and iron be greater than 90%; In mixed mineral powder, the mass fraction of sulfur-bearing is greater than 25%.
5. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaiming the method for copper, silver and iron, it is characterized in that, step 3) temperature of middle desulfurization with roasting technique is 850 ~ 950 DEG C.
6. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaim the method for copper, silver and iron, it is characterized in that, step 4) described in chlorinating agent be one in calcium chloride, sodium chloride or ammonium chloride.
7. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaim the method for copper, silver and iron, it is characterized in that, step 4) described in binding agent be one in bentonite or pellet binder.
8. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaim the method for copper, silver and iron, it is characterized in that, step 4) described in pelletizing diameter be 8 ~ 12mm.
9. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaim the method for copper, silver and iron, it is characterized in that, step 4) described in chloridising roasting temperature be 1000 ~ 1100 DEG C.
10. according to claim 1ly a kind ofly from zinc hydrometallurgy revolution kiln slag, reclaim the method for copper, silver and iron, it is characterized in that, step 4) described in the chloridising roasting time be 90 ~ 120min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105506298A (en) * | 2016-02-02 | 2016-04-20 | 广州中科正川环保科技有限公司 | Environment-friendly efficient resource recovery process for low-grade matte slag |
| CN107149979A (en) * | 2017-06-13 | 2017-09-12 | 汉源县伟业商贸有限公司 | A kind of method that iron is reclaimed in the revolution kiln slag from zinc hydrometallurgy |
| CN109266841A (en) * | 2018-11-27 | 2019-01-25 | 广东工业大学 | A kind of calcination process method of iron tailings |
| WO2019071791A1 (en) * | 2017-10-10 | 2019-04-18 | 东北大学 | Method for smelting reduction production of zinc smelting slag |
| CN110003968A (en) * | 2019-04-12 | 2019-07-12 | 隋有彬 | A kind of coal desulfurization device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105506298A (en) * | 2016-02-02 | 2016-04-20 | 广州中科正川环保科技有限公司 | Environment-friendly efficient resource recovery process for low-grade matte slag |
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| WO2019071791A1 (en) * | 2017-10-10 | 2019-04-18 | 东北大学 | Method for smelting reduction production of zinc smelting slag |
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| CN110003968A (en) * | 2019-04-12 | 2019-07-12 | 隋有彬 | A kind of coal desulfurization device |
| CN110003968B (en) * | 2019-04-12 | 2020-11-20 | 王天宇 | Coal desulfurization device |
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Application publication date: 20150429 |