CN102010994A - Iron depositing method of high acid and high iron solution goethite during zinc hydrometallurgy - Google Patents
Iron depositing method of high acid and high iron solution goethite during zinc hydrometallurgy Download PDFInfo
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Abstract
The present invention provides an iron depositing method of high acid and high iron solution goethite during zinc hydrometallurgy, comprising the following steps: a) carrying through oxidization leaching for zinc concentrate ore by using a sulphuric acid contained solution; b) reducing the leaching liquid by the zinc concentrated ore; c) pre-neutralizing the reduced liquid until pH value is 1.5-2.5, and generating a supernatant and a base flow via solid and liquid separation; d) carrying through goethite iron depositing for the generated supernatant, wherein after iron is deposited, liquid and solid are separated; the overflow is returned into a purification process; a part of the base flow is returned to a first iron depositing reactor as a seed crystal, and the rest base flow is discharged outwardly. The method provided by the present invention, iron is deposited in a form of goethite by using a high acid and high iron solution generated during zinc refining procedure; the grade of iron slag is high; and emissions of waste residues, waste gas and waste water are not increased.
Description
Technical field
The present invention relates to the Metal smelting field, be specifically related to the heavy iron method of peracid high iron solution pyrrhosiderite in a kind of zinc hydrometallurgy process.
Background technology
Since the seventies in last century, Zinc Hydrometallurgy Technology development rapidly, contrast pyrometallurgy of zinc, zinc hydrometallurgy have that labor condition is good, environmental protection, production are easy to serialization, automatization, maximize, be convenient to advantage such as comprehensive recovery, are generally adopted by each newly-built smeltery.
Traditional zinc hydrometallurgy process zinc ore concentrate need obtain zinc baking sand and sulfur dioxide flue gas through behind the fluidized bed roasting, though be used in relieving haperacidity through the flue gas after gathering dust, the tail gas after the relieving haperacidity still contains a certain amount of sulfurous gas, can cause topsoil.Along with the continuous development of Zinc Hydrometallurgy Technology, zinc ore concentrate need directly not leach the direct leaching-out technique that obtains solution of zinc sulfate through roasting and be adopted more and more.
Zinc ore concentrate utilizes peracid high temperature oxygen directly to leach, and iron content and vitriolic content are all very high in the solution of zinc sulfate that obtains, and iron is mainly with Fe
3+Form exists, and needs to sink iron before electric zinc technology, and adopts conventional heavy iron method deironing, and it is higher to contain zinc in the heavy scum, and the taste of iron is low, influences the resource utilization of iron.
Summary of the invention
The problem that the present invention solves is to provide a kind of method of zinc hydrometallurgy, can handle the peracid high iron solution that produces in the zinc metallurgy process, makes heavy scum ferrous grade height, can realize the resource utilization of iron.
In order to solve the problems of the technologies described above, technical scheme of the present invention is:
Peracid high iron solution pyrrhosiderite in a kind of zinc hydrometallurgy process sinks the iron method, may further comprise the steps:
A) zinc ore concentrate being used sulfur acid solution carry out oxidation leaches;
B) leach liquor reduces with zinc ore concentrate;
C) will going up after the reduction that the step produces liquid, to carry out pre-neutralization to pH value be 1.5～2.5, then through liquid-solid separation generation supernatant liquor and underflow;
D) supernatant liquor of Chan Shenging carries out the heavy iron of pyrrhosiderite, and (liquid carries out liquid-solid separation behind the heavy iron, and overflow enters cleaning section, and the underflow part is returned heavy iron reactor as crystal seed, and the rest part underflow effluxes.
As preferably, described a) in oxidation when leaching temperature be greater than 95 ℃, time 24h～32h, the terminal point acidity control is at 20～30g/l, mol ratio Fe
3+: Fe
2+=1～2: 1.
As preferably, described b) in during reduction temperature be 60 ℃～100 ℃, time 2h～4h.
As preferably, described c) carries out pre-neutralization for adding neutral leached mud, ZnO or the zinc baking sand that zinc hydrometallurgy produces.
As preferably, the time of pre-neutralization is 2h～3h, and temperature is 60 ℃～80 ℃.
As preferably, described underflow returns the oxidation that participates in zinc ore concentrate and leaches.
As preferably, described d) time of the heavy iron of pyrrhosiderite is 2h～4h in.
As preferably, the speed of response in the described heavy iron reactor is from slowly to soon.
As preferably, 5 heavy iron reaction units are set, the amount of oxygen in each heavy iron reaction unit is followed successively by 20m
3/ h～50m
3/ h, 50m
3/ h～150m
3/ h, 150m
3/ h～200m
3/ h, 200m
3/ h～300m
3/ h, 200m
3/ h～300m
3/ h.
As preferably, 5 heavy iron reaction units are set, use ZnO or zinc baking sand that the pH value in each heavy iron reaction unit is controlled to be 2.5～3.0,3.0～3.5,3.0～4.0,3.0～4.0,3.0～4.0 successively.
As preferably, described ZnO or zinc baking sand are by measuring belt blanking, described measuring belt and pH proofing unit interlocked control.
As preferably, the pyrrhosiderite in the described underflow returns as crystal seed and is used for the heavy iron of pyrrhosiderite, makes that to sink the concentration that contains crystal seed in the solution of iron be 50g/L～70g/L.
Peracid high iron solution pyrrhosiderite in the zinc hydrometallurgy process provided by the invention sinks the iron method, utilize reduction, pre-neutralization and heavy iron to handle the peracid high iron solution that produces in the zinc metallurgy process, scum is settled out, and scum is of high grade, can recycle realize the resource utilization of iron, the fluorine in can also adsorbent solution.The slag charge of reduction and pre-neutralization generation all returns the leaching operation of zinc ore concentrate in addition, has improved the leaching yield of zinc.Present method is simple to operate, does not increase the discharging of waste residue, waste gas and waste water.
Description of drawings
The schema of the Zinc hydrometallurgy process that Fig. 1 is provided for a kind of embodiment of the present invention.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
Please refer to Fig. 1, the schema of the Zinc hydrometallurgy process that Fig. 1 is provided for a kind of embodiment of the present invention.The method of zinc hydrometallurgy provided by the invention may further comprise the steps:
A) at first zinc ore concentrate is carried out the oxidation leaching in sulphuric acid soln, oxygen atmosphere and obtain solution of zinc sulfate, wherein the iron in the zinc ore concentrate is oxidized to Fe
3+Enter in the leach liquor, in addition the also residual sulfuric acid that higher concentration is arranged in the leach liquor.
B) with the high Fe of this peracid
3+Leach liquor reduce with zinc ore concentrate, stir, with Fe
3+Be reduced into Fe
2+, Fe
3+Amount be controlled in the 1g/L.Zinc sulphide in the zinc ore concentrate generates elemental sulfur and zine ion.Chemical equation is:
2Fe
3++ZnS＝Zn
2++2Fe
2++S (1)
Earlier according to Fe in the formula (1)
3+Amount calculate the amount of required ZnS, can obtain the amount of the zinc ore concentrate of required adding again according to the content of ZnS in the zinc ore concentrate.Temperature is 60 ℃～100 ℃ during preferred the reduction, time 2h～4h.
C) leach liquor being carried out pre-neutralization to pH value is 1.5～2.5, and neutral leached mud, ZnO or the zinc baking sand that can add conventional zinc hydrometallurgy generation carry out pre-neutralization, reduce the content of acid, obtain carrying out the qualified solution of the heavy iron of pyrrhosiderite.The time of preferred pre-neutralization is 2h～3h, and temperature is 60 ℃～80 ℃.Solution after the pre-neutralization produces supernatant liquor through dense back again and contains the underflow of slag charges such as zinc sulphide, zinc ferrite and elemental sulfur, supernatant liquor carries out the heavy iron of pyrrhosiderite, underflow is back to the oxidation of zinc ore concentrate and leaches operation, has improved the leaching yield of zinc, has also reduced the discharge of waste residue.And prior art is not carried out pre-neutralization, neutralizes in heavy iron process again, and the consumption of neutralizing agent increases when making heavy iron, causes that to contain zinc in the heavy scum too high, has reduced the taste of scum and has influenced its resource utilization.The oxidation leaching that the underflow after the reduction does not reflux and participates in zinc ore concentrate in the prior art in addition, but be used for burning the refining calcining.
D) supernatant liquor after the pre-neutralization carries out the heavy iron of pyrrhosiderite, remove the iron that contains in the solution in case do not influence zinc refinement and can be with iron resourcesization.The heavy iron of pyrrhosiderite utilizes dioxygen oxidation, with Fe
2+Oxidation generates FeOOH (pyrrhosiderite) precipitation.Need adding ZnO or zinc baking sand to control reaction pH value in the heavy iron process as neutralizing agent.Chemical equation is:
2Fe
2++1/2O
2+H
2O+2ZnO＝2FeOOH+2Zn
2+ (2)
The time of preferred heavy iron is 2h～4h.The requirement in the design consideration reaction times of heavy iron reactor is carried out, and speed of response is from slowly to soon.At least two heavy iron reactors of preferred setting, the amount of control oxygen and pH value are to increase gradually, and the heavy iron of slow oxidation can obtain sampling higher scum like this, and making heavy iron is pyrrhosiderite, is convenient to realize the resource utilization of iron.And conventional heavy iron process does not increase amount of oxygen gradually and improve the process of pH value gradually, and the heavy iron grade that obtains is low.
5 heavy iron reaction units preferably can be set, and the amount of oxygen in the heavy iron reaction unit of concrete each is followed successively by 20m
3/ h～50m
3/ h, 50m
3/ h～150m
3/ h, 150m
3/ h～200m
3/ h, 200m
3/ h～300m
3/ h, 200m
3/ h～300m
3/ h; Use ZnO or zinc baking sand that the pH value in each heavy iron reaction unit is controlled to be 2.5～3.0,3.0～3.5,3.0～4.0,3.0～4.0,3.0～4.0 successively.Preferably use zinc baking sand and do not use ZnO, ZnO contains Pb8%～15% than higher, can generate the galvanized iron vanadium if be used for heavy iron, can reduce the taste of iron in the heavy scum, be about 1.0%～2.0% and the content of Pb is relatively lower in the zinc baking sand, can reduce iron when being used for sinking iron and precipitate with galvanized iron vanadium form.Preferably when sinking iron, control the content of copper in the solution in addition greater than 0.3g/L.
Preferably by the measuring belt blanking, measuring belt and pH proofing unit interlocking carry out automatization control by detected pH value to the add-on of ZnO or zinc baking sand when adding ZnO or zinc baking sand, make heavy iron control more stable.
Solution behind the heavy iron carries out dense, the supernatant liquor that produces enters operation such as the neutrality leaching, electrodeposition of conventional zinc hydrometallurgy and obtains metallic zinc, contain heavy scum in the underflow, part is returned as the pyrrhosiderite crystal seed, make that to sink the concentration that contains crystal seed in the solution of iron be 50g/L～70g/L, the backflow crystal seed sinks iron can be accelerated iron in the solution and form goethite precipitation and get off.Remaining underflow effluxes.And conventional heavy iron method does not add crystal seed, and heavy iron effect is bad, the product potential difference of iron.
Effluxing has iron content to reach 37%～40% scum in the underflow, further resource utilization is as the raw material of ironmaking for the iron in the scum, and simultaneously the fluorine in the solution also is adsorbed and enters scum and efflux and be removed along with scum.
Embodiment 1:
A) adopt zinc ore concentrate to the high Fe of peracid
3+Leach liquor reduces.
The high Fe of peracid
3+The chemical ingredients of leach liquor is: Zn
2+138g/L, H
2SO
422g/L, Cu
2+1.1g/L, Fe
3+10g/L, Fe
2+6g/L.
The weight percent content of the zinc ore concentrate that adopts is: Zn41%, S32%, Fe8%.
Temperature is 80 ℃ during reduction, time 4h.
The chemical ingredients of the solution after the reduction that obtains is: Zn
2+145g/L, H
2SO
422g/L, Cu
2+1.1g/L, Fe
3+0.7g/L, Fe
2+14.7g/L.
B) leach liquor being carried out pre-neutralization to pH value is 1.5～2.5.
The neutral leached mud that adds conventional zinc hydrometallurgy generation carries out pre-neutralization to leach liquor, and the time of pre-neutralization is 3h, 80 ℃ of temperature.
The weight percent content of neutral leached mud is: Zn24%, Fe20%, Cu0.7%, S7%.
The chemical ingredients of the supernatant liquor that obtains after the pre-neutralization is: Zn
2+147g/L, Cu
2+1.3g/L, Fe
3+0.7g/L, Fe
2+14.7g/L, pH2.3.
C) supernatant liquor after the pre-neutralization is sunk iron.
The time of heavy iron is 4h, and the supernatant liquor flow is 110m
3/ h, reaction is provided with the heavy iron reaction tank of 5 20m * 3m * 1.5m.The amount of oxygen that feeds is 1# pond 40m
3/ h, 2# pond 100m
3/ h, 3# pond 180m
3/ h, 4# pond 240m
3/ h, 5# pond 280m
3/ h.
Use the ZnO calcining that the pH in the heavy iron process is controlled, the chemical ingredients of employed ZnO calcining is: Zn56%, Fe12%, Pb1.3%, Cu0.6%.The pH value once is controlled to be 1# pond 2.7,2# pond 3.2,3# pond 3.5,4# pond 3.6,5# pond 3.8.
The chemical ingredients of the supernatant liquor that obtains behind the heavy iron is: Zn
2+155g/L, Cu
2+1.8g/L, Fe
3+0.7g/L, Fe
2+0.24g/L, pH3.8.
The weight percent content of heavy scum is: Fe37%, Pb1.5%, Zn13%, Cu0.9%, F0.08%.
Embodiment 2:
A) adopt zinc ore concentrate to the high Fe of peracid
3+Leach liquor reduces.
The high Fe of peracid
3+The chemical ingredients of leach liquor is: Zn
2+132g/L, H
2SO
425g/L, Cu
2+1.3g/L, Fe
3+13g/L, Fe
2+3g/L.
The weight percent content of the zinc ore concentrate that adopts is: Zn41%, S32%, Fe8%.
Temperature is 100 ℃ during reduction, time 3h.
The chemical ingredients of the solution after the reduction that obtains is: Zn
2+138g/L, H
2SO
425g/L, Cu
2+1.3g/L, Fe
3+0.9g/L, Fe
2+14.3g/L.
B) leach liquor being carried out pre-neutralization to pH value is 1.5～2.5.
The neutral leached mud that adds conventional zinc hydrometallurgy generation carries out pre-neutralization to leach liquor, and the time of pre-neutralization is 3h, 70 ℃ of temperature.
The weight percent content of neutral leached mud is: Zn22%, Fe20%, Cu1.3%, S6.7%.
The chemical ingredients of the supernatant liquor that obtains after the pre-neutralization is: Zn
2+143g/L, Cu
2+1.5g/L, Fe
3+0.9g/L, Fe
2+14.3g/L, pH2.0.
C) supernatant liquor after the pre-neutralization is sunk iron.
The time of heavy iron is 3h, and the supernatant liquor flow is 100m
3/ h, reaction is provided with the heavy iron reaction tank of 4 20m * 2.5m * 1.5m.The amount of oxygen that feeds is 1# pond 50m
3/ h, 2# pond 100m
3/ h, 3# pond 150m
3/ h, 4# pond 200m
3/ h.
Use the ZnO calcining that the pH in the heavy iron process is controlled, the chemical ingredients of employed ZnO calcining is: Zn56%, Fe12%, Pb1.3%, Cu0.6%.The pH value once is controlled to be 1# pond 2.6,2# pond 3.3,3# pond 3.6,4# pond 3.8.
The chemical ingredients of the supernatant liquor that obtains behind the heavy iron is: Zn
2+156g/L, Cu
2+1.7g/L, Fe
3+0.7g/L, Fe
2+0.3g/L, pH3.8.
The weight percent content of heavy scum is: Fe35%, Pb1.7%, Zn14%, Cu0.9%, F0.06%.
More than the heavy iron method of the peracid high iron solution pyrrhosiderite in the zinc hydrometallurgy process provided by the present invention is described in detail.Used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (12)
1. the heavy iron method of the peracid high iron solution pyrrhosiderite in the zinc hydrometallurgy process is characterized in that, may further comprise the steps:
A) zinc ore concentrate being used sulfur acid solution carry out oxidation leaches;
B) leach liquor reduces with zinc ore concentrate;
C) will going up after the reduction that the step produces liquid, to carry out pre-neutralization to pH value be 1.5～2.5, then through liquid-solid separation generation supernatant liquor and underflow;
D) supernatant liquor of Chan Shenging carries out the heavy iron of pyrrhosiderite, and liquid carries out liquid-solid separation behind the heavy iron, and overflow enters cleaning section, and the underflow part is returned heavy iron reactor as crystal seed, and the rest part underflow effluxes.
2. method according to claim 1 is characterized in that, described a) in oxidation when leaching temperature be greater than 95 ℃, time 24h～32h, the terminal point acidity control is at 20～30g/l, mol ratio Fe
3+: Fe
2+=1～2: 1.
3. method according to claim 1 is characterized in that, described b) in when reduction temperature be 60 ℃～100 ℃, time 2h～4h.
4. method according to claim 1 is characterized in that, described c) be that neutral leached mud, ZnO or the zinc baking sand that adds the zinc hydrometallurgy generation carries out pre-neutralization.
5. method according to claim 4 is characterized in that, the time of pre-neutralization is 2h～3h, and temperature is 60 ℃～80 ℃.
6. method according to claim 5 is characterized in that, described underflow returns the oxidation that participates in zinc ore concentrate and leaches.
7. method according to claim 1 is characterized in that, described d) in time of the heavy iron of pyrrhosiderite be 2h～4h.
8. method according to claim 7 is characterized in that, the speed of response in the described heavy iron reactor is from slowly to soon.
9. method according to claim 8 is characterized in that, 5 heavy iron reaction units are set, and the amount of oxygen in each heavy iron reaction unit is followed successively by 20m
3/ h～50m
3/ h, 50m
3/ h～150m
3/ h, 150m
3/ h～200m
3/ h, 200m
3/ h～300m
3/ h, 200m
3/ h～300m
3/ h.
10. method according to claim 8 is characterized in that, 5 heavy iron reaction units are set, and uses ZnO or zinc baking sand that the pH value in each heavy iron reaction unit is controlled to be 2.5～3.0,3.0～3.5,3.0～4.0,3.0～4.0,3.0～4.0 successively.
11. method according to claim 10 is characterized in that, described ZnO or zinc baking sand are by measuring belt blanking, described measuring belt and pH proofing unit interlocked control.
12. method according to claim 1 is characterized in that, the pyrrhosiderite in the described underflow returns as crystal seed and is used for the heavy iron of pyrrhosiderite, makes that to sink the concentration that contains crystal seed in the solution of iron be 50g/L～70g/L.
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