CN104087754B - A kind of zinc ferrite calcination for activation-thing regulates and controls the method that zinc-iron separates mutually - Google Patents
A kind of zinc ferrite calcination for activation-thing regulates and controls the method that zinc-iron separates mutually Download PDFInfo
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Abstract
The invention discloses a kind of zinc ferrite calcination for activation-thing and regulate and control the method that zinc-iron separates mutually。Zinc ferrite class metallurgical slag adds ammonium sulfate, and 300-470 DEG C carries out calcination for activation and decompose zinc ferrite, and the thing of 480-670 DEG C of roasting regulation and control ferrum is Fe mutually2O3, in leaching process, zinc Selectively leaching obtains zinc-rich liquid, and ferrum is enriched in slag and obtains rich iron charge。Containing zinc 20g/L, iron content < 0.5g/L in zinc-rich liquid；Zinc leaching rate in optimal conditions > 92%, ferrum leaching rate < less than 0.8%；Zn content < 1% in rich iron charge, the slag rate that enters of ferrum reaches more than 99%。The present invention can reclaim zinc and ferrum in zinc ferrite class metallurgical waste effectively, has good economic implications and Significance for Environment。
Description
Technical field:
The invention belongs to metallurgical engineering and environmental project crossing domain, relate to a kind of zinc ferrite calcination for activation-thing and regulate and control the method that zinc-iron separates mutually, be specifically related to one and dregs containing zinc metallurgical slag is carried out zinc ferrite decomposition, the method that zinc-iron separates。
Background technology:
China is the first in the world Chan Xin big country, and zinc abstraction mainly adopts Zinc hydrometallurgy process, but Zinc hydrometallurgy process is when zinc concentrate oxidizing roasting, and the ferrum of association and zinc inevitably generate zinc ferrite。Zinc ferrite stable in properties, will not decompose when meutral innersion or Weak-acid leaching, causes that the zinc of about 20% is lost in leached mud, and the solution of the zinc ferrite produced for zinc abstraction technique at present mainly adopts pyrogenic process and wet processing to process。
Thermal process mainly adopts rotary kiln baking method, and zinc leaching residue allocates the coal dust of 30～40% into, reduces at 1100～1250 DEG C, and zinc is reduced, and enters fume recovery。This method energy consumption zinc product zinc oxide fumes high, that reclaim also to process further containing zinc about 45～60% and cause that in technological process length, zinc oxide fumes, fluorine-containing chlorine height affects zinc hydrometallurgy electrolytic deposition process。
Wet processing process mainly adopts hot acid to leach and makes major part zinc ferrite decomposition, but zinc and ferrum simultaneously enter leachate, leachate first carries out heavy ferrum and purifies and electrodeposition again, different heavy iron process produces different heavy scums, having iron vitriol slag, goethitum slag, bloodstone slag etc., the waste residue amount of generation is big, containing the ferrum of the zinc of more than 5% and more than 25% in slag, this part zinc and ferrum do not utilize, and cause substantial amounts of resources loss。Simultaneously possibly together with heavy metals such as lead, cadmiums in slag, the storing up serious harm environment and take substantial amounts of land resource of waste residue。The Zinc hydrometallurgy process of the oxygen leaching zinc concentrate of development in recent years, scum and leached mud that this technique produces still cannot utilize。
In recent years, substantial amounts of work has been done in decomposition for zinc ferrite, wet treatment aspect has pressure leaching, high temperature high acidic oils, pyrogenic process aspect have addition reducing agent high temperature reduction volatilize zinc, add volatilizer at high temperature strengthen volatilization zinc, middle temperature magnetizing roast decompose, middle temperature addition sodium carbonate, sodium hydroxide, sulfuric acid baking。Wet treatment zinc ferrite then zinc and ferrum leach in solution simultaneously, it does not have realize the separation of zinc and ferrum；High temperature reduction volatilize then temperature more than 1000 DEG C；Magnetizing roast is decomposed, ferrum zinc zinc possibly together with more than 10% in rich iron charge after separating；Zinc-rich liquid after sodium carbonate or the separation of sodium hydroxide roasting then zinc-iron has introduced substantial amounts of sodium ion；Sulfuric acid roasting method is the same with wet treatment zinc ferrite, and when leaching, zinc and ferrum are leached simultaneously, is not carried out zinc-iron and separates during leaching。
Patent (application number: 201410012237.1) discloses and a kind of add iron sulfate roasting-water logging and reclaim the method for zinc in dregs containing zinc waste residue, achieve the zinc-iron after zinc ferrite decomposes to separate, but separation efficiency still has much room for improvement, the material discomposing effect high particularly with dregs containing zinc is not as。
In sum, for zinc ferrite class metallurgical slag, the decomposition of zinc ferrite is separated with zinc-iron there is no good solution at present, cause that the zinc in waste residue, iron resource can not get effective utilization。Zinc ferrite is a difficult problem metallurgical and that environmental area is urgently to be resolved hurrily, in the urgent need to a kind of method finding effective decomposition zinc ferrite to realize zinc, ferrum separation and environmental protection。
Summary of the invention:
It is an object of the invention to for above-mentioned Problems existing, it is provided that a kind of zinc ferrite calcination for activation-thing regulates and controls the method that zinc-iron separates mutually。Can effectively decompose zinc ferrite, the thing of ferrum be regulated and controled mutually simultaneously, realize the high efficiency separation of zinc, ferrum at leaching process。
A kind of zinc ferrite calcination for activation-thing regulates and controls the method that zinc-iron separates mutually: zinc ferrite class metallurgical slag is added ammonium sulfate and carries out low-temperature activation roasting 30-60min at 300-470 DEG C, low-temperature activation roasting raises temperature after completing and carries out middle temperature thing to 480-670 DEG C and regulate and control roasting 15-45min mutually, finally realizes zinc-iron separation in leaching process。
In said method, the temperature of low-temperature activation roasting is preferably 300-400 DEG C。
The temperature that in said method, warm thing regulates and controls roasting mutually is preferably 500-650 DEG C。
It is preferred that 400 DEG C of low-temperature activation roasting 1h in said method, in 600 DEG C, temperature thing regulates and controls roasting 30min mutually。
Ammonium sulfate/zinc ferrite mass ratio=1～6 in said method。Ammonium sulfate/zinc ferrite mass ratio is preferably=2～6。
When leaching in said method, liquid-solid mass ratio is (5～20)/1。When preferably leaching, liquid-solid mass ratio is (5～8)/1。
Leaching agent used in leaching process in said method is pH is the aqueous solution of 2～7。
Extraction time at least 15 minutes in said method。
Dominant response in roasting process of the present invention is:
3(NH4)2SO4=4NH3+N2+3SO2(g)+6H2O(1)
ZnFe2O4+4SO2(g)+2O2(g)=ZnSO4+2Fe2(SO4)3(2)
Fe2(SO4)3=Fe2O3+3SO3(g)(3)
ZnSO4=ZnO+SO3(g)(4)
From accompanying drawing 1, in 300～670 DEG C of intervals, react the △ G < 0 of (1), (2), (3), the △ G > 0 of reaction (4), illustrate in this temperature range, reaction (1), (2), (3) all can carry out, and reaction (4) will not carry out。Accompanying drawing 2 it can be seen that fired slags XRD figure in have zinc sulfate and iron sesquioxide, it does not have zinc oxide thing phase, further illustrate reaction (1), (2), (3) occur, reaction (4) do not occur。
As: when carrying out roasting for 400 DEG C, Decomposition of ammonium sulfate, produce sulfur dioxide gas；Newly generated sulfur dioxide reacts generation iron sulfate by reaction (2) and zinc ferrite。Owing to material is mixed homogeneously before roasting with ammonium sulfate, ammonium sulfate decomposes generation sulfur dioxide at the particle surface of material, sulfur dioxide participates in the decomposition reaction of zinc ferrite immediately at particle surface, greatly reduces the time of the bulk diffusion entrance internal batch of gas-solid reaction seasonal epidemic pathogens；Moreover sulfur dioxide produces on material surface, can be fully contacted with material particles surface, considerably increase response area；In addition newly-generated sulfur dioxide gas more reactivity。Therefore, zinc ferrite is carried out calcination for activation by the present invention under cryogenic, it is achieved that the efficient-decomposition of zinc ferrite。With the acid leaching residue of dregs containing zinc 64.97% for raw material, process by sulfuric acid roasting method and iron sulfate roasting method, more under equal conditions Leaching Zinc, see following table with Comparative result of the present invention:
Table 1 the inventive method and sulfuric acid baking, iron sulfate roasting method Comparative result
| Method of roasting | Zinc ferrite resolution ratio % | Zinc ferrite % in fired slags | Zinc leaching rate % |
| Sulfuric acid baking | 59.07 | 5.75 | 70.35 |
| Iron sulfate roasting | 65.36 | 5.21 | 71.52 |
| The inventive method | 80.29 | 2.46 | 91.52 |
From table 1, compared with sulfuric acid roasting method and iron sulfate roasting method, in fired slags of the present invention, the content of zinc ferrite reduces 57.21% and 52.78%；Application the inventive method, zinc ferrite resolution ratio and zinc leaching rate all improve more than 23%。
Iron sulfate can be decomposed into sulfur trioxide and iron sesquioxide when more than 480 DEG C, and zinc sulfate decomposition temperature is at 680 DEG C。Therefore when 480～670 DEG C of roastings, iron sulfate reacts by reaction (3), changes and generates iron sesquioxide, but the thing of zinc sulfate will not change mutually。From accompanying drawing 1, as temperature < 670 DEG C, zinc sulfate decomposition reaction △ G > 0, understand that zinc sulfate does not now decompose in theory；From accompanying drawing 2, after roasting, in fired slags, the thing of zinc is zinc sulfate mutually, and the thing that experimental result describes at roasting process zinc sulfate does not change mutually。
When leaching, zinc sulfate is dissolved in neutrality～slightly acidic water solution, and iron sesquioxide is insoluble, stays slag phase。Isolated by filtration can obtain zinc-rich liquid and rich iron charge, and in zinc-rich liquid, iron content is low, low containing zinc in rich iron charge。
From XRD figure in accompanying drawing 2, the dominant in raw material is zinc ferrite mutually, and in fired slags, dominant is zinc sulfate and iron sesquioxide mutually, illustrates that zinc ferrite generates zinc sulfate and iron sulfate through Roasting Decomposition, and iron sulfate is iron sesquioxide through Roasting Decomposition；In leached mud, dominant is iron sesquioxide mutually, illustrates that zinc sulfate has leached in solution。
In sum, the invention has the beneficial effects as follows: sintering temperature is low, zinc ferrite decomposition temperature is 300～470 DEG C；The thing carrying out ferrum while Roasting Decomposition zinc ferrite regulates and controls mutually, achieves zinc, ferrum separation at leaching process；In roasting process, principal solid product is zinc sulfate and iron sesquioxide, it does not have introduce foreign ion；Compared with sulfuric acid roasting method, sulfuric acid roasting method sintering temperature is 250～270 DEG C, sintering temperature of the present invention is 300～470 DEG C, although sintering temperature of the present invention is high, but after the present invention is regulated and controled mutually by thing, leaching process achieves zinc-iron separate, and in fired slags of the present invention, the content of zinc ferrite reduces 57.21%；Compared with iron sulfate roasting method, iron sulfate roasting method sintering temperature is 500～1000 DEG C, and sintering temperature of the present invention is lower, and in fired slags of the present invention, the content of zinc ferrite reduces 52.78%。
Accompanying drawing illustrates:
Fig. 1 is thermodynamic advantages administrative division map of the present invention；
Fig. 2 is raw material of the present invention, fired slags, rich scum XRD figure。
Detailed description of the invention:
Below in conjunction with specific embodiment, the present invention being described in further details, specific embodiment described herein is only used for explaining the present invention, is not limited to the present invention。
Embodiment 1:
Accounting for more than 90% by levigate for the acid leaching residue 100g of dregs containing zinc to-200 orders (74um), the content of Zn and Fe respectively 17.73% and 21.91% in acid leaching residue, zinc ferrite content is 11.52%, accounts for total zinc 64.97%。Allocate 25g ammonium sulfate mix homogeneously into, 400 DEG C of roasting 1h, then by roasting furnace temperature elevation to 600 DEG C roasting 30min, take out cooling。
Fired slags water extraction, room temperature, leachate pH is 5, and liquid-solid ratio is 6/1, and extraction time 15min has leached rear isolated by filtration, obtains zinc-rich liquid and rich scum。Containing zinc 19.7g/L in zinc-rich liquid, iron content is 0.31g/L；Zinc leaching rate is 91.52%, and ferrum leaching rate is 0.8%；Containing zinc 1.96%, ferrum 42.10% in rich scum。
Embodiment 2:
Accounting for more than 90% by levigate for the mixing slag 100g of dregs containing zinc to-200 orders (74um), the content of Zn and Fe respectively 14.96% and 23.06% in slag, zinc ferrite content is 5.76%。Allocate 20g ammonium sulfate mix homogeneously into, 400 DEG C of roasting 1h, then by roasting furnace temperature elevation to 600 DEG C roasting 30min, take out cooling。
Fired slags water extraction, room temperature, leachate pH is 7, and liquid-solid ratio is 8/1, and extraction time 15min has leached rear isolated by filtration, obtains zinc-rich liquid and rich scum。Containing zinc 18.05g/L in zinc-rich liquid, iron content is 0.24g/L；Zinc leaching rate is 87.25%, and ferrum leaching rate is 0.57%；Containing zinc 2.37%, ferrum 48.07% in rich scum。
Embodiment 3:
Accounting for more than 90% by levigate for the goethitum slag 100g of dregs containing zinc to-200 orders (74um), the content of Zn and Fe respectively 9.56% and 35.42% in slag, zinc ferrite content is 5.52%。Allocate 30g ammonium sulfate mix homogeneously into, 400 DEG C of roasting 1h, then by roasting furnace temperature elevation to 600 DEG C roasting 30min, take out cooling。
Fired slags water extraction, room temperature, leachate pH is 7, and liquid-solid ratio is 5/1, and extraction time 20min has leached rear isolated by filtration, obtains zinc-rich liquid and rich scum。Containing zinc 23.51g/L in zinc-rich liquid, iron content is 0.46g/L；Zinc leaching rate is 92.76%, and ferrum leaching rate is 0.81%；Containing zinc 1.82%, ferrum 57.03% in rich scum。
Embodiment 4:
Accounting for more than 90% by levigate for the goethitum slag 100g of dregs containing zinc to-200 orders (74um), the content of Zn and Fe respectively 9.56% and 35.42% in slag, zinc ferrite content is 5.52%。Allocate 30g ammonium sulfate mix homogeneously into, 350 DEG C of roasting 60min, then by roasting furnace temperature elevation to 650 DEG C roasting 15min, take out cooling。
Fired slags water extraction, room temperature, leachate pH is 7, and liquid-solid ratio is 5/1, and extraction time 20min has leached rear isolated by filtration, obtains zinc-rich liquid and rich scum。Containing zinc 23.18g/L in zinc-rich liquid, iron content is 0.56g/L；Zinc leaching rate is 91.52%, and ferrum leaching rate is 0.99%；Containing zinc 1.96%, ferrum 56.82% in rich scum。
Embodiment 5:
Accounting for more than 90% by levigate for the goethitum slag 100g of dregs containing zinc to-200 orders (74um), the content of Zn and Fe respectively 9.56% and 35.42% in slag, zinc ferrite content is 5.52%。Allocate 30g ammonium sulfate mix homogeneously into, 450 DEG C of roasting 30min, then by roasting furnace temperature elevation to 500 DEG C roasting 45min, take out cooling。
Fired slags water extraction, room temperature, leachate pH is 7, and liquid-solid ratio is 5/1, and extraction time 20min has leached rear isolated by filtration, obtains zinc-rich liquid and rich scum。Containing zinc 22.87g/L in zinc-rich liquid, iron content is 14.16g/L；Zinc leaching rate is 90.55%, and ferrum leaching rate is 24.94%；Containing zinc 2.57%, ferrum 43.26% in rich scum。
From above example, the inventive method effectively achieves zinc-iron Selective Separation in leaching process, and under optimum condition, zinc leaching rate is 87～93%, and the leaching rate of ferrum is below 0.8%；The slag rate that enters of ferrum reaches more than 99%。By rich scum is processed the rich iron charge that can obtain zinc content < 1% further。
Claims (10)
1. zinc ferrite calcination for activation-thing regulates and controls the method that zinc-iron separates mutually, it is characterized in that: zinc ferrite class metallurgical slag is added ammonium sulfate and carries out low-temperature activation roasting 30-60min at 300-470 DEG C, low-temperature activation roasting raises temperature after completing and carries out middle temperature thing to 480-670 DEG C and regulate and control roasting 15-45min mutually, finally realizes zinc-iron separation in leaching process。
2. zinc ferrite calcination for activation-thing according to claim 1 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: the temperature of low-temperature activation roasting is 300-400 DEG C。
3. zinc ferrite calcination for activation-thing according to claim 1 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: middle temperature thing regulates and controls the temperature of roasting mutually and is 500-650 DEG C。
4. zinc ferrite calcination for activation-thing according to claim 1 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: 400 DEG C of low-temperature activation roasting 1h, in 600 DEG C, temperature thing regulates and controls roasting 30min mutually。
5. the zinc ferrite calcination for activation-thing according to claim 1 or 2 or 3 or 4 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: ammonium sulfate/zinc ferrite mass ratio=1～6。
6. zinc ferrite calcination for activation-thing according to claim 5 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: ammonium sulfate/zinc ferrite mass ratio=2～6。
7. the zinc ferrite calcination for activation-thing according to claim 1 or 2 or 3 or 4 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: during leaching, liquid-solid mass ratio is (5～20)/1。
8. zinc ferrite calcination for activation-thing according to claim 7 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: during leaching, liquid-solid mass ratio is (5～8)/1。
9. the zinc ferrite calcination for activation-thing according to claim 1 or 2 or 3 or 4 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: leaching agent used in leaching process is pH is the aqueous solution of 2～7。
10. the zinc ferrite calcination for activation-thing according to claim 1 or 2 or 3 or 4 regulates and controls the method that zinc-iron separates mutually, it is characterised in that: extraction time is 15min at least。
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| CN104178642B (en) * | 2014-08-31 | 2015-12-09 | 中南大学 | A kind of method of zinc and iron in separation of Zinc leached mud |
| CN105063365B (en) * | 2015-09-11 | 2017-03-22 | 中南大学 | Method for efficiently decomposing zinc ferrite in metallurgical waste slag. |
| CN105331801B (en) * | 2015-11-27 | 2017-07-18 | 中南大学 | A kind of zinc concentrate cooperates with method of roasting with pyrite |
| CN109852811A (en) * | 2019-02-26 | 2019-06-07 | 武汉科技大学 | A kind of zinc-iron efficient separation method |
| CN110863219B (en) * | 2019-12-04 | 2021-04-16 | 北京环丁环保大数据研究院 | Method for resource utilization of zinc-containing converter dust and sludge |
| CN113528854A (en) * | 2021-07-23 | 2021-10-22 | 昆明冶金研究院有限公司 | Method for extracting zinc from oxygen-sulfur mixed lead-zinc ore |
| CN113881852B (en) * | 2021-09-09 | 2023-04-11 | 重庆大学 | Method for one-step recovery and separation of zinc and iron from electric furnace dust |
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