CN105112676B - A kind of method of pyrite roasting fayalite class metallurgical slag recovery iron - Google Patents

A kind of method of pyrite roasting fayalite class metallurgical slag recovery iron Download PDF

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CN105112676B
CN105112676B CN201510568445.4A CN201510568445A CN105112676B CN 105112676 B CN105112676 B CN 105112676B CN 201510568445 A CN201510568445 A CN 201510568445A CN 105112676 B CN105112676 B CN 105112676B
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pyrite
iron
roasting
metallurgical slag
class metallurgical
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CN105112676A (en
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彭兵
柴立元
李燕春
袁莹珍
刘恢
闵小波
彭宁
雷杰
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Central South University
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Abstract

The invention discloses a kind of method of pyrite roasting fayalite class metallurgical slag recovery iron.Fayalite class metallurgical slag adds pyrite, is leached after 300 1100 DEG C carry out oxidizing roasting, then with acid solution, iron leaching rate>94%, or high intensity magnetic separation is carried out, iron content reaches 66% in magnetic concentrate.The present invention can be calcined the iron effectively reclaimed in fayalite class metallurgical slag and pyrite cinder by pyrite autothermal oxidation, and the minimizing and recycling effect for fayalite class metallurgical slag and pyrite cinder are obvious.

Description

A kind of method of pyrite roasting fayalite class metallurgical slag recovery iron
Technical field：
The invention belongs to metallurgical engineering and environmental project crossing domain, and it is metallurgical to be related to a kind of pyrite roasting fayalite class The method that waste residue reclaims iron, and in particular to a kind of that roasting recovery iron is carried out to the fayalite class metallurgical slag such as lead skim, copper ashes, nickel slag Method.
Background technology：
China is the first in the world steel big producer, but China's iron ore deposit is poor, and substantial amounts of iron ore deposit is by external Import, China's iron ore rely on import continuous 6 years more than 60%.At the same time, China produces a large amount of metallurgical slags every year, The substantial amounts of iron resource of association in these metallurgical slags.Wherein Copper making industry produces millions of tons of copper ashes every year, iron content in copper ashes 40%；Lead smelting industry produces millions of tons of lead skims every year, iron content 21-31% in lead skim；Nickel fibers industry produces hundreds of every year Ten thousand tons of nickel slags, nickel slag iron content 30-40%.These slags are largely stored up at present, cause environmental pollution and the wasting of resources.Recovery copper ashes, Minimizing and iron resource of the iron resource for metallurgical slag, make up China in the fayalite class metallurgical slag such as lead skim, nickel slag The chronic shortage of iron ore resource is significant.
The recovery of iron mainly obtains iron ore concentrate by oxidation/reduction roasting-magnetic separation, directly gone back in copper ashes, lead skim, nickel slag Original-magnetic separation obtains iron ore concentrate, Direct Reductive Melting obtains ferroalloy.Iron is mainly with fayalite thing phase in copper ashes, lead skim, nickel slag In the presence of.Fayalite property is stable, carries out oxidizing roasting with oxygen below 1000 DEG C or carries out reduction roasting with carbon monoxide/carbon Burn, fayalite is converted into the iron of four oxidation two or the conversion ratio of di-iron trioxide is not high, therefore oxidation/reduction roasting-magnetic separation It is undesirable to handle fayalite class metallurgical slag effect, iron does not have concentration effect when particularly handling lead skim.Direct-reduction-magnetic separation Substantial amounts of coal is then added, in 1000-1200 DEG C of reduction, Direct Reductive Melting is reduced under conditions of 1400 DEG C of ＞, energy Consumption is high.Fayalite does not dissolve in diluted acid, can not directly leach, and after using concentrated acid pulp, is just dissolved under conditions of strong acid high temperature.
In summary, the recycling of iron resource lacks effective method in fayalite class metallurgical slag at present so that Iron resource cannot get effective recycling in these metallurgical slags.The recycling of iron resource is in fayalite class metallurgical slag Metallurgical and environmental area problem urgently to be resolved hurrily, there is an urgent need to a kind of energy-conservation, the process that efficient, flow is short to reclaim iron olive The iron resource of association in stone class metallurgical slag.
The content of the invention:
The purpose of the present invention is to be directed to above-mentioned problem, there is provided a kind of pyrite roasting fayalite class metallurgical slag The method for reclaiming iron.By adding pyrite roasting by fayalite thing phase decomposition in waste residue, then the side by leaching or magnetic separation Formula reclaims iron.
A kind of method of pyrite roasting fayalite class metallurgical slag recovery iron：One in optional following two schemes Kind：
(1) fayalite class metallurgical slag adds pyrite, is calcined under aerobic conditions, by fired slags acid after the completion of roasting Solution is leached to obtain iron content leachate, or fired slags progress high intensity magnetic separation is obtained into iron ore concentrate；
(2) fayalite class metallurgical slag is added into pyrite two sections of low-temperature bakes in oxidizing atmosphere, fired slags are with weak After the valuable metals such as Ore Leaching zinc-copper lead, then with acid solution leach to obtain iron content leachate or carry out high intensity magnetic separation to obtain iron ore concentrate.
Sintering temperature is 300-1100 DEG C in scheme (1), and preferably 450-900 DEG C of roasting time is 15-180min, preferably 60-90min。
Two sections of low-temperature bakes refer to 300-600 DEG C of roasting 30-150min, preferably 30-90min in scheme (2), then in 600- 700 DEG C of roastings 30-150min, preferably 30-60min.
Weight of iron ratio=1~8 in above-mentioned pyrite/fayalite class metallurgical slag.
Weight of iron ratio preferably 1~3 in above-mentioned pyrite/fayalite class metallurgical slag.
Oxygen concentration in two schemes is 1-100%, and preferably 100%.
The sulfuric acid that the acid solution of leaching iron is 20-98% in two schemes, 8-38% hydrochloric acid, 14-69% nitric acid, 12-56% acetic acid it is any；It is preferred that 30-50% sulfuric acid, 12-19% hydrochloric acid, 20-35% nitric acid, 15-28%'s Acetic acid；The solid mass ratio of leachate is (5~20)/1, preferably (5~10)/1；1~60min of extraction time；Extraction temperature 25-100 ℃。
In scheme (2) weak acid solution of leaching valuable metal be sulfur acid, hydrochloric acid, nitric acid it is any, concentration range is 0.1-5%；The solid mass ratio of leachate is (5~20)/1；1~60min of extraction time；25-100 DEG C of extraction temperature；Weak-acid leaching Liquid adds zinc dust precipitation recovery zinc-copper lead valuable metal after carrying out circulating leaching.
The magnetic field intensity that fired slags carry out high intensity magnetic separation in two schemes is the Gausses of 1.0-1.6 ten thousand, preferably 1.2 ten thousand Gausses.
Described fayalite class metallurgical slag includes lead skim, copper ashes or nickel slag.
The chemical reaction process of oxidation of pyrite burning of the present invention is as follows：
2FeS2+5.5O2→Fe2O3+3SO2(g) (1)
2FeS2+7O2→Fe2(SO4)3+SO2(g) (2)
FeS2+3O2→FeSO4+4SO2(g) (3)
The chemical reaction process that oxidation of pyrite combustion intermediate product ferric sulfate and ferrous sulfate of the present invention decompose It is as follows：
Fe2(SO4)3→Fe2O3+3SO3(g) (4)
2FeSO4→Fe2O3+SO3(g)+SO2(g) (5)
2FeSO4+1/2O2(g)→Fe2O3+2SO3(g) (6)
The chemical reaction that sulfur dioxide of the present invention decomposes various Fe clusters in waste residue is as follows：
Fe3O4+SO2(g)+O2(g)→Fe2(SO4)3 (7)
Fe2O3+SO2(g)+O2(g)→Fe2(SO4)3 (8)
FeO+SO2(g)+O2(g)→Fe2(SO4)3 (9)
Fe+SO2(g)+O2(g)→Fe2(SO4)3 (10)
2FeO·SiO2+SO2(g)+O2(g)→Fe2(SO4)3+SiO2 (11)
FeO·SiO2+SO2(g)+O2(g)→Fe2(SO4)3+SiO2 (12)
The chemical reaction of various Fe clusters is as follows in sulphur trioxide decomposition waste residue of the present invention：
Fe3O4+SO3(g)→Fe2(SO4)3+SO2(g) (13)
Fe2O3+SO3(g)→Fe2(SO4)3 (14)
FeO+SO3(g)→Fe2(SO4)3+SO2(g) (15)
Fe+SO3(g)→Fe2(SO4)3+SO2(g) (16)
2FeO·SiO2+SO3(g)→Fe2(SO4)3+SiO2 (17)
FeO·SiO2+SO3(g)→Fe2(SO4)3+SiO2 (18)
As 500 DEG C of sintering temperature ＞, Fe clusters reaction product ferric sulfate is decomposed into di-iron trioxide in waste residue：
Fe2(SO4)3→Fe2O3+3SO3(g) (19)
In the first sets of plan of the invention, iron mainly mutually exists with fayalite thing in fayalite class metallurgical slag, this There are a small amount of metallic iron, ferroso-ferric oxide (Fe outside3O4), di-iron trioxide (Fe2O3), ferrous oxide (FeO).Pyrite is pressed React (1)-(3) and carry out oxidizing fire reaction, release sulfur dioxide (SO2), while oxidation of pyrite combustion intermediate product sulfuric acid Iron and ferrous sulfate decompose release sulfur dioxide (SO by (4)-(6)2) and sulfur trioxide (SO3).Intermediate gaseous product sulfur dioxide It is ferric sulfate (Fe by (7)-(12) are reacted by the thing phase decomposition of various iron in waste residue2(SO4)3), sulfur trioxide by reaction (13)- (18) it is ferric sulfate (Fe by the thing phase decomposition of various iron in waste residue2(SO4)3).As 500 DEG C of sintering temperature ＞, iron is anti-in waste residue The product ferric sulfate that should be obtained can be decomposed into di-iron trioxide by reaction (19).From above-mentioned course of reaction, pyrite is added Fayalite class metallurgical slag is calcined, Fe clusters are ferric sulfate or di-iron trioxide in the fired slags finally given.Can be to roasting Slag carries out Ore Leaching extraction iron or obtains iron ore concentrate to fired slags progress high intensity magnetic separation.
It is all when fayalite class metallurgical slag is being calcined for 300-600 DEG C in the second sets of plan of the invention Fe clusters can be converted into ferric sulfate.Zinc, copper and lead can be separately converted to zinc sulfate, copper sulphate and lead sulfate in waste residue.Again will be useless When being calcined for 600-700 DEG C, zinc sulfate and lead sulfate do not convert slag, and copper sulphate is converted into cupric oxide, and ferric sulfate is converted into Di-iron trioxide, therefore zinc, copper and lead etc. in waste residue can be extracted in advance with weak-acid leaching, separated with iron.Weak-acid leaching liquid enters After row circulating leaching, the valuable metals such as the recyclable lead of zinc dust precipitation, zinc, copper are added.
Pyrite is mainly used in oxidizing roasting relieving haperacidity.After oxidation of pyrite roasting, substantial amounts of pyrite cinder, Huang Tie are produced Main iron content in ore deposit slag, simultaneously containing valuable metals such as lead, copper, zinc.Pyrite cinder is mainly stored up at present, both to environment Harm is produced, causes the wasting of resources again.With oxidation of pyrite roasting fayalite class metallurgical slag recovery iron resource, roasting process Reacted after element sulphur oxidation in middle pyrite with iron in metallurgical slag and lead, zinc, copper etc., ferro element is then and metallurgical in pyrite Ferro element simultaneously participates in reaction in waste residue, is extracted in leaching process or during magnetic separation.Therefore it is calcined with oxidation of pyrite Fayalite class metallurgical slag can not only reclaim iron resource in fayalite class metallurgical slag, realize fayalite class metallurgical slag Recycling and minimizing, while the iron resource in pyrite cinder can also be reclaimed, realize minimizing and the money of pyrite cinder Source, reduce environmental pressure.Method provided by the invention can use oxidation of pyrite Roasting Decomposition metallurgical slag below 1000 DEG C Middle fayalite, iron or the means enriched iron with high intensity magnetic separation can be extracted with acid solution after roasting.
In summary, the beneficial effects of the invention are as follows：It can be calcined the mutually effectively conversion of fayalite thing below 1000 DEG C； Carbon or coal need not be added, and oxidation of pyrite roasting process heat release, energy consumption are low；Technological process is short；It is simple to operate；It can reclaim simultaneously Iron in pyrite cinder and fayalite class metallurgical slag；Separate and reclaim pyrite cinder and fayalite class is metallurgical useless The valuable metals such as zinc, copper, lead in slag；Fired slags have a wide range of application, available for preparing various iron salt solutions, it can also be used to refine Iron.
Brief description of the drawings：
Fig. 1 is present invention process flow chart.
Embodiment：
The present invention is described in further details with reference to specific embodiment, specific embodiment described herein is only used In explaining the present invention, it is not intended to limit the invention.
Embodiment 1：
More than 90% is accounted for -200 mesh (74um) by lead skim and pyrite are levigate, and Fe content is 23.84% in lead skim.Press Pyrite and lead skim are well mixed by weight of iron ratio for 2/1 in pyrite/lead skim, oxygen concentration 100%, 450 DEG C of roastings 90min, after the completion of roasting, the fired slags of pyrite and lead skim mixture are taken out and cooled down.
Fired slags are leached with 18% hydrochloric acid solution, 80 DEG C, liquid-solid ratio 10/1, extraction time 15min, mistake after the completion of leaching Filter separation.It is 94.25% to be calcined slag iron leaching rate.
Embodiment 2：
More than 90% is accounted for -200 mesh (74um) by lead skim and pyrite are levigate, and Fe content is 23.84% in lead skim.Press Pyrite and lead skim are well mixed by weight of iron ratio for 2/1 in pyrite/lead skim, oxygen concentration 100%, 800 DEG C of roastings 60min, after the completion of roasting, the fired slags of pyrite and lead skim mixture are taken out and cooled down.Fired slags carry out high intensity magnetic separation, and magnetic field is strong Spend for 1.2 ten thousand Gausses, iron content is 65.13% in magnetic separation of iron ore concentrate.
Contrast experiment 1 (lead skim oxidizing roasting-magnetic separation recovery iron)：By lead skim it is levigate to -200 mesh (74um) account for 90% with On, Fe content is 23.84% in lead skim.Lead skim is passed through to 2% oxygen, 800 DEG C of oxidizing roasting 30min, after being calcined, taken Go out cooling, magnetic separation is carried out under conditions of magnetic field intensity is 0.116T, iron content is 25.4% in magnetic separation of iron ore concentrate.
Contrast experiment 2 (lead skim reduction roasting-magnetic separation recovery iron)：By lead skim it is levigate to -200 mesh (74um) account for 90% with On, Fe content is 23.84% in lead skim.Lead skim is passed through to 5% CO, 800 DEG C of reduction roasting 60min, after being calcined, taken out Cooling, magnetic separation is carried out under conditions of magnetic field intensity is 0.116T, iron content is 35.86% in magnetic separation of iron ore concentrate.
Embodiment 3：
More than 90% is accounted for -200 mesh (74um) by copper ashes and pyrite are levigate, and Fe content is 40.54% in copper ashes.Press Pyrite and copper ashes are well mixed by weight of iron ratio for 3/1 in pyrite/copper ashes, oxygen concentration 100%, 700 DEG C of roastings 90min, after the completion of roasting, the fired slags of pyrite and copper ashes mixture are taken out and cooled down.
Fired slags carry out high intensity magnetic separation, and magnetic field intensity be 1.2 ten thousand Gausses, and iron content is 66.25% in magnetic separation of iron ore concentrate.Implement Example 4：
Nickel sizing is carefully accounted for more than 90% to -200 mesh (74um), Fe content is 35.26% in nickel slag.By pyrite/ Pyrite and nickel slag are well mixed by weight of iron than 3/2 in nickel slag, oxygen concentration 100%, 1000 DEG C of roasting 60min, have been calcined Cheng Hou, the fired slags of pyrite and nickel slag mixture are taken out and cooled down.
Fired slags are leached with 40% sulfuric acid solution, and extraction temperature is 80 DEG C, liquid-solid ratio 10/1, extraction time 20min, leaching It is separated by filtration after the completion of going out.Iron leaching rate is 93.72%.
Embodiment 5：
More than 90% is accounted for -200 mesh (74um) by lead skim is levigate, and Fe content is 23.84% in lead skim.By pyrite/ Pyrite and lead skim are well mixed by weight of iron than 3/1 in lead skim, oxygen concentration 100%, 500 DEG C of roasting 60min, then 650 DEG C roasting 60min, after the completion of roasting, by the fired slags of pyrite and lead skim mixture take out cool down.
Fired slags are pre-processed with 5% salt Ore Leaching.After 5% hydrochloric acid leachate carries out circulating leaching, zinc is added Powder substitution reclaims lead and zinc.
High intensity magnetic separation is carried out after fired slags pretreatment, and magnetic field intensity is 1.2 ten thousand Gausses, and iron content is in magnetic separation of iron ore concentrate 66.75%, Zn content ＜ 1%, lead content ＜ 0.5% in iron ore concentrate.
Embodiment 6：
More than 90% is accounted for -200 mesh (74um) by copper ashes is levigate, and Fe content is 40.54% in copper ashes.By pyrite/ Pyrite and copper ashes are well mixed by weight of iron than 3/1 in copper ashes, 400 DEG C of roasting 60min, oxygen concentration 100%.Again 600 DEG C roasting 60min, after the completion of roasting, by the fired slags of pyrite and copper ashes mixture take out cool down.
Fired slags are leached with 2% nitric acid and pre-processed.After 2% leaching solution carries out circulating leaching, zinc is added Powder substitution reclaims copper.
High intensity magnetic separation is carried out after fired slags pretreatment, and magnetic field intensity is 1.2 ten thousand Gausses, and iron content is in magnetic separation of iron ore concentrate 66.82%, copper content ＜ 0.5% in iron ore concentrate.
From above example, the inventive method uses pyrite roasting fayalite class metallurgical slag below 900 DEG C, After the fired slags of pyrite and fayalite class metallurgical slag mixture leach, iron leaching rate ＞ 94%, after magnetic separation in iron ore concentrate Iron content illustrates that the present invention can effectively reclaim iron in pyrite and fayalite class metallurgical slag more than 66%.Two sections of combination roastings After burning weak-acid leaching pretreatment, Zn content can be reduced to 1% in iron ore concentrate, lead content ＜ 0.5%, copper content ＜ 0.5%, weak acid Leachate carry out circulating leaching after be used for reclaim lead, zinc, copper, illustrate the inventive method can also efficiently separate and reclaim pyrite with Lead, zinc, copper etc. in fayalite class metallurgical slag.Iron content leachate can be used for preparing various ferrites or flocculant, magnetic separation essence Ore deposit can be used as iron-smelting raw material.

Claims (10)

  1. A kind of 1. method of pyrite roasting fayalite class metallurgical slag recovery iron, it is characterised in that optional following two sides One kind in case：
    (1) fayalite class metallurgical slag adds pyrite, is calcined under aerobic conditions, by fired slags acid solution after the completion of roasting Leached to obtain iron content leachate, or fired slags progress high intensity magnetic separation is obtained into iron ore concentrate；
    (2) fayalite class metallurgical slag addition pyrite two sections of low-temperature bakes, fired slags in oxidizing atmosphere are soaked with weak acid After going out zinc-copper lead valuable metal, then with acid solution leach to obtain iron content leachate or carry out high intensity magnetic separation to obtain iron ore concentrate；
    Sintering temperature is 300-1100 DEG C in scheme (1), roasting time 15-180min；
    Two sections of low-temperature bakes refer to 300-600 DEG C of roasting 30-150min in scheme (2), then are calcined 30- at 600-700 DEG C 150min；
    Weight of iron ratio=1~8 in pyrite/fayalite class metallurgical slag；
    Oxygen concentration in two schemes is 1-100%.
  2. 2. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 1, it is characterised in that： Sintering temperature is that 450-900 DEG C of roasting time is 60-90min in scheme (1).
  3. 3. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 1, it is characterised in that： Two sections of low-temperature bakes refer to 300-600 DEG C of roasting 30-90min in scheme (2), then are calcined 30-60min at 600-700 DEG C.
  4. 4. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 1, it is characterised in that： Weight of iron ratio in pyrite/fayalite class metallurgical slag is 1~3.
  5. 5. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 1, it is characterised in that： The sulfuric acid that the acid solution of leaching iron is 20-98% in two schemes, 8-38% hydrochloric acid, 14-69% nitric acid, 12-56%'s Acetic acid it is any；The solid mass ratio of leachate is (5~20)/1；1~60min of extraction time；25-100 DEG C of extraction temperature.
  6. 6. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 5, it is characterised in that： The sulfuric acid that the acid solution of leaching iron is 30-50% in two schemes, 12-19% hydrochloric acid, 20-35% nitric acid, 15-28%'s Acetic acid；The solid mass ratio of leachate is (5~10)/1.
  7. 7. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 1, it is characterised in that： The weak acid solution of leaching valuable metal is sulfur acid, hydrochloric acid, any, concentration range 0.1-5% of nitric acid in scheme (2)； The solid mass ratio of leachate is (5~20)/1；1~60min of extraction time；25-100 DEG C of extraction temperature；Weak-acid leaching liquid is followed Ring adds zinc dust precipitation recovery zinc-copper lead valuable metal after leaching.
  8. 8. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 1, it is characterised in that： The magnetic field intensity that fired slags carry out high intensity magnetic separation in two schemes is the Gausses of 1.0-1.6 ten thousand.
  9. 9. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 8, it is characterised in that： The magnetic field intensity that fired slags carry out high intensity magnetic separation in two schemes is 1.2 ten thousand Gausses.
  10. 10. the method for pyrite roasting fayalite class metallurgical slag recovery iron according to claim 1, its feature exist In：Described fayalite class metallurgical slag includes lead skim, copper ashes or nickel slag.
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CN115386722A (en) * 2022-08-30 2022-11-25 苏州金之翼新材料科技有限公司 Method for separating rare earth and iron from pyrite roasting neodymium iron boron waste

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