CN114622086A - Method for integrated treatment of milling, roasting and sorting of lean oxidized ore - Google Patents
Method for integrated treatment of milling, roasting and sorting of lean oxidized ore Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/10—Roasting processes in fluidised form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
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- B03D2201/00—Specified effects produced by the flotation agents
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Abstract
The invention discloses a method for integrated processing of milling, roasting and sorting of lean oxidized ore, relates to the technical field of lean oxidized ore processing, and particularly relates to a method for integrated processing of milling, roasting and sorting of lean oxidized ore, which comprises the following steps: s1, dry milling; s2, suspension magnetization roasting; s3, grinding and magnetically separating; s4, and carrying out reverse flotation and defluorination. Compared with the traditional magnetizing roasting technology, the method has the advantages that the material is in a fluidized state and runs in the system in the suspension magnetizing roasting process, and the heat and mass transfer efficiency is higher; the technology can realize the accurate control of various iron minerals in the magnetizing roasting process, finally generate the ferromagnetic gamma-Fe 2O3 with lower coercive force, and simultaneously can recover sensible heat and latent heat in the cooling process, thereby obviously reducing the energy consumption; meanwhile, after the artificial magnetite is converted into the gamma-Fe 2O3, the occurrence of the magnetic agglomeration phenomenon can be obviously reduced, and the quality of the iron ore concentrate is obviously improved.
Description
Technical Field
The invention relates to the technical field of lean oxide ore treatment, in particular to a method for integrally treating lean oxide ore by milling, roasting and sorting.
Background
The existing middle-lean oxidized piled ore of Baiyunebo is ore which is collected and abandoned and piled in a mine when steel is coated in a furnace for smelting in 1959 to 1964, the iron content of the ore is 20 to 33 percent, the average grade is 25 to 30 percent, the content of rare earth oxide is about 5.5 percent, the content of fluorite is more than 20 percent, the ore type is complex, the ore belongs to refractory middle-lean oxidized ore, and the ore piling amount is about 1500 ten thousand tons. The ore has the advantages of deeper oxidation degree and longer stacking time, the physical and chemical properties of the surface of the ore are greatly changed after long-term weathering, water immersion and oxidation, great difficulty is brought to sorting, and good technical and economic indexes cannot be obtained by adopting the conventional ore dressing technology. Meanwhile, the stacking ore occupies a large area, and the mineral elements in the ore can be migrated to the nearby ground surface and underground water due to overlong stacking time, so that soil pollution and water pollution are caused, and a large environmental protection risk exists.
The magnetizing roasting is the most effective pretreatment technology for treating complex and refractory iron ores, and the developing of the magnetizing roasting equipment with high production efficiency, stable operation and low energy consumption becomes a common target of mining science and technology and industry. Magnetizing roasting refers to heating the material or ore in a corresponding atmosphere to perform a chemical reaction, so as to make hematite (Fe) therein2O3) Siderite (FeCO)3) Limonite (Fe)2O3·nH2O) or other weakly magnetic iron mineral into strongly magnetic magnetite (Fe)3O4) Or maghemite (gamma-Fe)2O3). Common magnetizing roasting modes include shaft roasting, rotary kiln roasting, fluidized roasting and the like.
In application, the existing magnetizing roasting technology has a plurality of problems. Vertical furnace magnetizing roastingThe sintering process is mainly suitable for processing lump ores with the granularity of 15-75mm, and has the problems of low single-machine processing capacity, high energy consumption, long sintering time, uneven product quality and the like. At present, only a wine steel selection burning factory in China adopts 44 seats of 100m3Roasting the specularia type iron ore in a shaft furnace. The rotary kiln magnetizing roasting process is suitable for treating ores with the granularity of below 25mm, and the magnetizing roasting quality and the sorting index are better than those of a shaft furnace. In the major western ditch concentrating mill, siderite is treated by adopting a coal-based rotary kiln magnetization roasting-low intensity magnetic separation-reverse flotation process, and an industrial production index of 60.63% of TFe grade of iron concentrate and 75.42% of iron recovery rate is obtained. However, the rotary kiln process still has the problems of low magnetic susceptibility, easy ring formation, unstable production, low operation rate, high energy consumption and the like.
In recent years, a great deal of research is carried out by many domestic research units aiming at fluidization magnetizing roasting technology and equipment. However, the following problems are present:
1) a plurality of iron minerals are magnetized synchronously, and the reaction difference is large and the effect is poor;
2) the heating and the reduction of the materials are carried out in the same furnace chamber, the reducing atmosphere is weak, and the efficiency is low;
3) the artificial magnetite has large coercive force and slightly poor magnetic separation index, and latent heat cannot be efficiently recovered in the cooling process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for the integrated treatment of milling, roasting and sorting of lean oxidized ores, which solves the problems in the background art.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for carrying out milling, roasting and sorting integrated treatment on lean oxidized ore comprises the following steps:
s1, dry milling: crushing the medium-lean oxidized ore with the granularity of 5-40 mm to be less than 1mm through a high-pressure roller;
s2, suspension magnetization roasting: feeding ore is a dry-method powder-making product, which keeps a suspension state in the whole suspension magnetizing roasting process and carries out three-stage treatment;
s201, a first stage: firstly, pre-oxidizing mineral powder in an oxidizing atmosphere at the temperature of 650-700 ℃;
s202, a second stage: carrying out heat storage reduction roasting on the product subjected to the pre-oxidation operation in a reducing atmosphere at the temperature of 500-600 ℃;
s203, a third stage: the heat-accumulating reduction roasting product is cooled to 180-250 ℃ under the protection of nitrogen, the iron phase does not change at the stage, and then the heat-accumulating reduction roasting product is contacted with air and Fe2O3Reacting with oxygen in the air to generate ferromagnetic mineral-gamma-Fe 2O3 with low coercive force, and releasing latent heat at the same time, at the stage, recovering sensible heat and latent heat in the cooling and reoxidation process, and returning the preheated gas to the main furnace to support combustion or preheat materials;
s3, grinding and magnetically separating;
s4, defluorination by reverse flotation: feeding ore is magnetic concentrate, ore pulp with the weight percentage concentration of 35-42% is added into a flotation machine to carry out two-stage closed-loop operation of 'primary rough concentration and primary fine concentration'.
Optionally, in the step S1, the iron grade of the lean oxidized ore in the dry milling is 25-30%.
Optionally, in the step S201, in the first stage, various types of iron minerals such as hematite, goethite, limonite, siderite and magnetite in the ore are converted into Fe with uniform components2O3. The main reactions that occur are as follows:
Fe2O3·nH2O→α-Fe2O3+nH2O(g)
4FeCO3+O2→2α-Fe2O3+4CO2
4Fe3O4+O2→6α-Fe2O3。
optionally, in the step S202 and the second stage, a mixed gas of nitrogen and reducing gas in a ratio of 2: 1-4: 1 is introduced into the furnace body, and the specific ratio is according to Fe in the complex ore2O3The content is determined, and the main reactions are as follows:
3Fe2O3+CO→2Fe3O4+CO2
3Fe2O3+H2→2Fe3O4+H2O。
optionally, the main reactions in the step S203 and the third stage are as follows:
4Fe3O4+O2→6γ-Fe2O3。
optionally, in the step S3 and the ore grinding magnetic separation, the method specifically includes the following steps:
s301, feeding ore which is a roasted product, and stirring, grinding and fine grinding the roasted product to a particle size range of 70-90% below 0.074 mm;
s302, carrying out low-intensity magnetic separation with the magnetic field intensity of 1200-1600 Oe, separating out magnetic iron minerals in the roasted product, and enabling the magnetic separation tailings rich in rare earth to enter a process for recovering rare earth.
Optionally, in the step S4, in the rough flotation defluorination process, a collector, an inhibitor and an ore pulp pH regulator are selected, the flotation temperature is 35-40 ℃, the flotation time is 4-7min, the flotation tailings are removed, and the flotation concentrate enters the concentration process;
and in the fine selection, adding 50-200 g/t of sodium oleate serving as a collecting agent again, wherein the fine selection concentrate is the final iron concentrate, and the fine selection tailings are returned to the rough selection for re-selection.
Optionally, the collecting agent is sodium oleate with the dosage of 200-800 g/t, the inhibitor is water glass with the dosage of 600-1100 g/t, and the ore pulp pH regulator is sodium carbonate and sulfuric acid with the pH value of 7.5-8.
The invention provides a method for carrying out milling, roasting and sorting integrated treatment on lean oxidized ore, which has the following beneficial effects:
the invention adopts the high-pressure roller dry method for preparing powder, and carries out multi-material layer crushing on the material, so that microcracks in particles are increased, the particle strength is reduced, and the follow-up ore grinding operation is facilitated.
Compared with the traditional magnetizing roasting technology, the method has the advantages that the material is in a fluidized state and runs in the system in the suspension magnetizing roasting process, and the heat and mass transfer efficiency is higher; the technology can realize the accurate control of various iron minerals in the magnetizing roasting process, finally generate the ferromagnetic gamma-Fe 2O3 with lower coercive force, and simultaneously can recover sensible heat and latent heat in the cooling process, thereby obviously reducing the energy consumption; meanwhile, after the artificial magnetite is converted into the gamma-Fe 2O3, the occurrence of the magnetic agglomeration phenomenon can be obviously reduced, and the quality of the iron ore concentrate is obviously improved.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
S1, dry milling: crushing the lean oxide ore blocks in Baiyunebo with the granularity of 5-40 mm to below 1mm by a high-pressure roller; the iron grade of the medium lean oxidized ore is 28%;
s2, suspension magnetization roasting: feeding ore is a dry-method powder-making product, and the ore is kept in a suspension state in the whole suspension magnetizing roasting process;
s201, a first stage: the mineral powder is first pre-oxidized in the oxidizing atmosphere at about 680 deg.c to convert various kinds of iron mineral, such as goethite, limonite, siderite, magnetite, etc. into Fe with homogeneous component2O3The main reactions that take place are as follows:
Fe2O3·nH2O→α-Fe2O3+nH2O(g)
4FeCO3+O2→2α-Fe2O3+4CO2
4Fe3O4+O2→6α-Fe2O3;
s202, a second stage: the product of the pre-oxidation operation is subjected to heat storage reduction roasting at the temperature of 550 ℃, and nitrogen and reducing gas (CO and H) with the ratio of 3.5:1 are introduced into the furnace body2Or coal gas) mixed gas, the main reactions taking place are as follows:
3Fe2O3+CO→2Fe3O4+CO2
3Fe2O3+H2→2Fe3O4+H2O;
s203, a third stage: cooling the heat-storage reduction roasting product to 190 ℃ under the protection of nitrogen, and contacting air to obtain Fe3O4Oxidizing to generate ferromagnetic mineral-gamma-Fe with low coercive force2O3And simultaneously recovering sensible heat and latent heat in the cooling reoxidation process, wherein the main reactions are as follows:
4Fe3O4+O2→6γ-Fe2O3;
s3, grinding and magnetic separation: finely grinding the roasted product by adopting a stirring mill to a particle size range of 85 percent below 0.074mm, and then carrying out low intensity magnetic separation with the magnetic field intensity of 1500Oe to separate magnetic iron minerals in the roasted product;
s4, defluorination by reverse flotation: preparing ore pulp with the weight percentage concentration of 40 percent, adding the ore pulp into a flotation machine to perform two-stage closed-loop operation of primary rough concentration and primary fine concentration;
in the rough concentration, selecting sodium oleate (the dosage of 500g/t) as a collecting agent, water glass (the dosage of 800g/t) as an inhibitor, sodium carbonate and sulfuric acid as an ore pulp pH regulator (the pH value is 8), the flotation temperature is 39 ℃, the flotation time is 5min, removing flotation tailings, and selecting flotation concentrate;
and in the fine flotation, 120g/t of sodium oleate is added again to serve as a collecting agent, the fine flotation concentrate is the final iron concentrate, the fine flotation tailings are returned to the rough flotation for re-flotation, and the final iron concentrate with the iron grade of 64.9% and the iron recovery rate of 81.2% is obtained through defluorination of the magnetic concentrate through reverse flotation.
Example 2
S1, dry milling: crushing the bayan obo lean oxidized ore blocks with the granularity of 5-40 mm to below 1mm by a high-pressure roller; the iron grade of the medium lean oxidized ore is 26%;
s2, suspension magnetization roasting: feeding ore is a dry-method powder-making product, and the ore is kept in a suspension state in the whole suspension magnetizing roasting process;
s201, a first stage: the ore powder is first pre-oxidized in oxidizing atmosphere at 660 deg.c to obtain goethite, limonite and sideriteConversion of various types of iron minerals such as ore and magnetite into Fe with uniform components2O3The main reactions that take place are as follows:
Fe2O3·nH2O→α-Fe2O3+nH2O(g)
4FeCO3+O2→2α-Fe2O3+4CO2
4Fe3O4+O2→6α-Fe2O3;
s202, a second stage: the product of the pre-oxidation operation is subjected to heat storage reduction roasting at the temperature of 550 ℃, and nitrogen and reducing gas (CO and H) with the ratio of 4:1 are introduced into the furnace body2Or coal gas) mixed gas. The main reactions that take place are as follows:
3Fe2O3+CO→2Fe3O4+CO2
3Fe2O3+H2→2Fe3O4+H2O;
s203, a third stage: cooling the heat-accumulating reduction roasting product to 230 ℃ under the protection of nitrogen, and contacting with air to obtain Fe3O4Oxidizing to generate ferromagnetic mineral-gamma-Fe with low coercive force2O3And simultaneously recovering sensible heat and latent heat in the cooling reoxidation process, wherein the main reactions are as follows:
4Fe3O4+O2→6γ-Fe2O3;
s3, grinding and magnetic separation: finely grinding the roasted product by adopting a stirring mill to a particle size range of less than 0.074mm and accounting for 81%, and then carrying out low intensity magnetic separation with the magnetic field intensity of 1200Oe to separate out magnetic iron minerals in the roasted product;
s4, defluorination by reverse flotation: preparing ore pulp with the weight percentage concentration of 37 percent, adding the ore pulp into a flotation machine to perform two-stage closed-loop operation of primary rough concentration and primary fine concentration;
in the rough concentration, selecting sodium oleate (dosage of 300g/t) as a collecting agent, water glass (dosage of 900g/t) as an inhibitor, sodium carbonate and sulfuric acid as an ore pulp pH regulator (pH is 8), carrying out flotation at the temperature of 37 ℃ for 5min, removing flotation tailings, and carrying out concentration on flotation concentrates;
and in the fine selection, 100g/t of sodium oleate is added again to serve as a collecting agent, the fine selection concentrate is the final iron concentrate, the fine selection tailings are returned to the rough selection for re-selection, and the magnetic separation concentrate is defluorinated through reverse flotation to obtain the final iron concentrate with the iron grade of 65.1% and the iron recovery rate of 80.4%.
Example 3
S1, dry milling: crushing the lean oxide ore blocks in Baiyunebo with the granularity of 5-40 mm to below 1mm by a high-pressure roller; the iron grade of the medium lean oxidized ore is 30 percent;
s2, suspension magnetization roasting: feeding ore is a dry-method powder-making product, and the ore is kept in a suspension state in the whole suspension magnetizing roasting process;
s201, in the first stage, the mineral powder is firstly pre-oxidized in an oxidizing atmosphere with the temperature of about 690 ℃, and in the first stage, various types of iron minerals such as goethite, limonite, siderite and magnetite in the mineral are converted into Fe with uniform components2O3The main reactions that take place are as follows:
Fe2O3·nH2O→α-Fe2O3+nH2O(g)
4FeCO3+O2→2α-Fe2O3+4CO2
4Fe3O4+O2→6α-Fe2O3;
s202, in the second stage, the product of the pre-oxidation operation is subjected to heat storage reduction roasting at the temperature of 520 ℃ in a reducing atmosphere, and nitrogen and reducing gas (CO and H) with the ratio of 2.5:1 are introduced into the furnace body2Or coal gas), the main reactions that take place are as follows:
3Fe2O3+CO→2Fe3O4+CO2
3Fe2O3+H2→2Fe3O4+H2O;
s203, in the third stage, the heat storage reduction roasting product is cooled to 240 ℃ under the protection of nitrogen and then contacts with air, and Fe3O4Oxidizing to generate ferromagnetic mineral-gamma-Fe with low coercive force2O3And simultaneously recovering sensible heat and latent heat in the cooling reoxidation process, wherein the main reactions are as follows:
4Fe3O4+O2→6γ-Fe2O3;
s3, grinding and magnetic separation: finely grinding the roasted product by adopting a stirring mill to a particle size range of 75% below 0.074mm, and then carrying out low intensity magnetic separation with the magnetic field intensity of 1400Oe to separate out magnetic iron minerals in the roasted product;
s4, defluorination by reverse flotation: preparing ore pulp with the weight percentage concentration of 42 percent, adding the ore pulp into a flotation machine to perform two-stage closed-loop operation of primary rough concentration and primary fine concentration;
in the rough concentration, selecting sodium oleate (the dosage of 600g/t) as a collecting agent, water glass (the dosage of 1000g/t) as an inhibitor, sodium carbonate and sulfuric acid as an ore pulp pH regulator (the pH value is 8), the flotation temperature is 37 ℃, the flotation time is 7min, removing flotation tailings, and selecting flotation concentrate;
and in the fine selection, 130g/t of sodium oleate is added again to serve as a collecting agent, the fine selection concentrate is the final iron concentrate, the fine selection tailings are returned to the rough selection for re-selection, and the magnetic separation concentrate is defluorinated through reverse flotation to obtain the final iron concentrate with the iron grade of 64.6% and the iron recovery rate of 82.1%.
In summary, the method for the integrated processing of milling, roasting and sorting of the lean oxidized ore adopts the suspension magnetization roasting technology, and the lean oxidized ore is processed by the steps of pre-oxidation, heat storage reduction roasting and reoxidation, and a plurality of iron minerals are oxidized into hematite (alpha-Fe) with uniform components2O3) And reducing the hematite into ferromagnetic magnetite (Fe)3O4) Finally low-temperature oxidation to stronger magnetic hematite (gamma-Fe)2O3) And latent heat is released, so that the precise regulation and control of the iron mineral in the roasting process are realized, and the Fe can be treated in the reoxidation stage after the roasting is finished3O4→γ-Fe2O3Sensible heat and latent heat in the process are recovered, energy consumption is obviously reduced, and meanwhile, artificial magnetite is converted into gamma-Fe2O3Then, the occurrence of magnetic agglomeration phenomenon can be obviously reduced, and the ironThe quality of the concentrate is obviously improved; finally, a key technology of 'dry milling, suspension magnetization roasting, ore grinding, magnetic separation and flotation' of lean ores is formed, the sorting index that the iron grade of the iron ore concentrate is greater than 64.5% and the recovery rate is greater than 80% is obtained, and technical support is provided for efficient development and utilization of the lean ores.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (8)
1. A method for the integrated treatment of milling, roasting and sorting of lean oxidized ores comprises the following steps:
s1, dry milling: crushing the medium-lean oxidized ore with the granularity of 5-40 mm to be less than 1mm through a high-pressure roller;
s2, suspension magnetization roasting: feeding ore is a dry-method powder-making product, which keeps a suspension state in the whole suspension magnetizing roasting process and carries out three-stage treatment;
s201, a first stage: firstly, pre-oxidizing mineral powder in an oxidizing atmosphere at the temperature of 650-700 ℃;
s202, a second stage: carrying out heat storage reduction roasting on the product subjected to the pre-oxidation operation in a reducing atmosphere at the temperature of 500-600 ℃;
s203, a third stage: the heat-storage reduction roasting product is cooled to 180-250 ℃ under the protection of nitrogen, the iron phase does not change at the stage, and then the heat-storage reduction roasting product is contacted with air and Fe2O3Reacting with oxygen in the air to generate ferromagnetic mineral-gamma-Fe 2O3 with low coercive force, and releasing latent heat at the same time, at the stage, recovering sensible heat and latent heat in the cooling and reoxidation process, and returning the preheated gas to the main furnace to support combustion or preheat materials;
s3, grinding and magnetically separating;
s4, defluorination by reverse flotation: feeding ore is magnetic concentrate, ore pulp with the weight percentage concentration of 35-42% is added into a flotation machine to carry out two-stage closed-loop operation of 'primary rough concentration and primary fine concentration'.
2. The method for integrated processing of milling, roasting and sorting of the lean oxidized ore according to claim 1, characterized in that: and S1, the iron grade of the lean oxidized ore in the dry powder preparation is 25-30%.
3. The method of claim 1, wherein in step S201, the first stage, the hematite, goethite, limonite, siderite and magnetite of various types of iron minerals in the ore are converted into Fe with uniform components2O3. The main reactions that occur are as follows:
Fe2O3·nH2O→α-Fe2O3+nH2O(g)
4FeCO3+O2→2α-Fe2O3+4CO2
4Fe3O4+O2→6α-Fe2O3。
4. the method for integrated processing of milling, roasting and sorting of the lean oxidized ore according to claim 1, characterized in that in the step S202 and the second stage, a mixed gas of nitrogen and reducing gas is introduced into the furnace body in a ratio of 2: 1-4: 1, wherein the specific ratio is determined according to Fe in the complex ore2O3The content is determined, and the main reaction is as follows:
3Fe2O3+CO→2Fe3O4+CO2
3Fe2O3+H2→2Fe3O4+H2O。
5. the method for integrated processing of milling, roasting and sorting of oxide-deficient ore according to claim 1, wherein the main reactions in the step S203 and the third stage are as follows:
4Fe3O4+O2→6γ-Fe2O3。
6. the method for integrated processing of milling, roasting and sorting of the lean oxidized ore according to claim 5, wherein the step S3 and the ore grinding magnetic separation specifically comprise the following steps:
s301, feeding ore which is a roasted product, and stirring, grinding and fine grinding the roasted product to a particle size range of 70-90% below 0.074 mm;
s302, carrying out low-intensity magnetic separation with the magnetic field intensity of 1200-1600 Oe, separating out magnetic iron minerals in the roasted product, and enabling the magnetic separation tailings rich in rare earth to enter a process for recovering rare earth.
7. The method for integrated processing of milling, roasting and sorting of the lean oxidized ore according to claim 1, characterized in that in the step S4, during the defluorination and flotation, a collector, an inhibitor and a pulp pH regulator are selected, the flotation temperature is 35-40 ℃, the flotation time is 4-7min, the flotation tailings are removed, and the flotation concentrate enters the concentration;
and in the fine selection, adding 50-200 g/t of sodium oleate serving as a collecting agent again, wherein the fine selection concentrate is the final iron concentrate, and the fine selection tailings are returned to the rough selection for re-selection.
8. The method for integrated processing of milling, roasting and sorting of the lean oxidized ore according to claim 7, characterized in that: the collecting agent is sodium oleate with the dosage of 200-800 g/t, the inhibitor is water glass with the dosage of 600-1100 g/t, and the ore pulp pH regulator is sodium carbonate and sulfuric acid with the pH value of 7.5-8.
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