CN112458276A - Method for preparing iron ore concentrate and sulfur by synergistic treatment of iron-containing tailings and pyrite - Google Patents
Method for preparing iron ore concentrate and sulfur by synergistic treatment of iron-containing tailings and pyrite Download PDFInfo
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- CN112458276A CN112458276A CN202011179111.5A CN202011179111A CN112458276A CN 112458276 A CN112458276 A CN 112458276A CN 202011179111 A CN202011179111 A CN 202011179111A CN 112458276 A CN112458276 A CN 112458276A
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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
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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
- B03C1/005—Pretreatment specially adapted for magnetic separation
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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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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a method for preparing iron ore concentrate and sulfur by synergistic treatment of iron-containing tailings and pyrite, which comprises the following steps: mixing the iron-containing tailings with pyrite; and (3) carrying out high-temperature roasting treatment on the mixture under the protection of inert gas, cooling gas generated by high-temperature roasting, cooling to obtain a solid product, namely sulfur, and carrying out magnetic separation on roasted slag obtained by roasting to obtain iron ore concentrate and magnetic separation tailings. According to the invention, the iron-containing tailings and the pyrite are cooperatively treated, so that the iron-containing tailings can promote sulfur in the pyrite to be converted into sulfur, and iron contained in the iron-containing tailings and the pyrite can be converted into ferroferric oxide which is easy to separate by magnetic separation, thereby solving the problems of iron-containing tailings generated by smelting enterprises and pyrite generated by mineral processing enterprises and pollution to the surrounding environment.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of tailing resources, and particularly relates to a method for preparing iron ore concentrate and sulfur by synergistic treatment of iron-containing tailings and pyrite.
Background
A large amount of iron-containing tailings are generated in industries such as acid making, smelting and the like in China, most of the iron-containing tailings generated at present are in a stockpiling state, resource utilization cannot be achieved, a large amount of land is occupied, surface and underground water systems are polluted, and serious threats are brought to ecological environment and resident health.
Pyrite is the most widespread sulphide mineral present in the crust, often associated with non-ferrous sulphide minerals. In order to extract target metal in the non-ferrous metal smelting process, pyrite is often stockpiled or sent to acid-making enterprises as a by-product in the dressing and smelting process, and the stockpiling not only occupies a large amount of land, but also has certain influence on the surrounding environment due to the characteristics of the pyrite; in addition, the sulfuric acid production capacity is surplus in China, and the application of pyrite to acid making is not a good choice.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art, and provide a method for preparing iron ore concentrate and sulfur by the synergistic treatment of iron-containing tailings and pyrite.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing iron ore concentrate and sulfur by the synergistic treatment of iron-containing tailings and pyrite comprises the following steps:
(1) mixing the iron-containing tailings with pyrite;
(2) carrying out high-temperature roasting treatment on the mixture obtained in the step (1) under the protection of inert gas, cooling gas generated by high-temperature roasting, and cooling to obtain a solid product, namely sulfur;
(3) and (3) carrying out magnetic separation on the roasting slag obtained by roasting in the step (2) to obtain iron ore concentrate and magnetic separation tailings.
As described abovePreferably, in the step (1), the addition amount of the iron-containing tailings and the pyrite is 0.2-0.5 mol of iron disulfide per mol of iron trioxide based on the iron trioxide in the iron-containing tailings and the iron disulfide in the pyrite. The excessive addition of pyrite can form pyrrhotite (Fe)7S8) The magnetic iron enters magnetite in the magnetic separation process, so that the magnetite contains sulfur and is not beneficial to the subsequent iron smelting; if the addition amount of pyrite is too small, Fe cannot be added2O3Reduction to Fe3O4(the main reaction involved is FeS2+4Fe2O3=3Fe3O4+S2(g) And even cause side reactions resulting in low sulfur conversion.
Preferably, in the step (2), the high-temperature roasting temperature is 500-1000 ℃, and the high-temperature roasting time is not less than 20 min.
In the above method, preferably, in the step (2), the cooled gas is recycled.
In the above method, preferably, in the step (2), before the high-temperature roasting treatment, inert gas is introduced into the roasting furnace, and air is exhausted to form an inert atmosphere in the furnace. Furthermore, the volume of the introduced inert gas is 2-6 times of the internal volume of the hearth.
In the method, preferably, in the step (2), the inert gas is continuously introduced into the reaction furnace during the high-temperature roasting treatment, and the rate of continuously introducing the inert gas is not lower than 10 mL/min.
Preferably, in the step (3), the calcine slag is ground before magnetic separation, and the ground ore has an ore grain size of-0.075 mm accounting for 85-90%.
In the above method, preferably, in the step (3), the magnetic field strength for magnetic separation is 100 to 200 kA.m-1。
In the method, the iron-containing tailings are preferably produced from smelting tailings obtained by smelting enterprises, wherein the main iron-containing component of the smelting tailings is Fe2O3The pyrite component mainly contains FeS2。
Compared with the prior art, the invention has the advantages that:
(1) according to the invention, the iron-containing tailings and the pyrite are subjected to synergistic treatment, the iron-containing tailings can promote sulfur in the pyrite to be converted into sulfur, and iron contained in both the iron-containing tailings and the pyrite can be converted into ferroferric oxide which is easy to separate by magnetic separation.
(2) The invention processes the iron-containing tailings and the pyrite cooperatively, prepares iron ore concentrate and sulfur products simultaneously, has the advantages of high resource utilization rate, obvious slag reduction, good environmental protection benefit and the like, and simultaneously the magnetic separation tailings are mainly substances such as silicon dioxide and the like and can be used as auxiliary materials for production of building materials and the like.
(3) The invention has the advantages of short process flow, low cost, high resource utilization rate, obvious slag reduction and the like.
(4) The invention solves the problems of iron-containing tailings produced by smelting enterprises and pyrite produced by mineral processing enterprises in stockpiling and pollution to the surrounding environment.
Drawings
FIG. 1 is an XRD pattern of iron-containing tailings # 1 employed in examples of the present invention.
Fig. 2 is an XRD pattern of iron-containing tailings # 2 employed in examples of the present invention.
Fig. 3 is an XRD pattern using pyrite in the example of the present invention.
FIG. 4 is an XRD pattern of sulfur obtained in example 1 of the present invention.
Fig. 5 is an XRD pattern of iron ore concentrate obtained in example 1 of the present invention.
FIG. 6 is a photograph of sulfur obtained in example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The iron-containing tailings used in the following examples have the compositions shown in table 1, the phase analyses shown in fig. 1 and 2, the compositions of pyrites used in table 2, and the phase analyses shown in fig. 3.
Table 1: chemical composition of iron-containing tailings
Name of material | S(%) | Fe(%) | Zn(%) | SiO2 | Pb(%) | Cu(%) |
Iron-containing |
0.72 | 47.82 | 1.06 | 25.49 | 1.01 | 0.11 |
Iron-containing |
1.14 | 34.60 | 0.56 | 39.25 | 0.44 | 0.32 |
Table 2: chemical composition of pyrite
Name (R) | Fe | S | SiO2 |
Mass fraction (%) | 43.36 | 45.26 | 4.63 |
Example 1:
the invention discloses a method for preparing iron ore concentrate and sulfur by the synergistic treatment of iron-containing tailings and pyrite, which comprises the following steps:
(1) 1000g of iron-containing tailings # 1 and 135g of pyrite (molar ratio Fe)2O3:FeS21:0.25) and uniformly mixing to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a tubular furnace, and slowly introducing nitrogen into the furnace (the introduction amount of the nitrogen is 3 times of the volume of a hearth) to exhaust air in the furnace; starting heating, continuously introducing nitrogen at the speed of 100mL/min, heating to 800 ℃, keeping the temperature, roasting for 1.5h, discharging and cooling gas generated in the roasting process to separate out sulfur in the gas to obtain 58g of sulfur, wherein the picture is shown in FIG. 6, and the cooled gas is pumped to an inert gas vent and is continuously introduced into the furnace to realize recycling;
(3) after the furnace temperature is reduced to 50 ℃, stopping introducing nitrogen, taking out the roasted slag, grinding the roasted slag until the fineness is minus 0.075mm and accounting for 85 percent, and performing magnetic separation, wherein the strength used for the magnetic separation is 150 kA.m-1And carrying out magnetic separation to obtain iron ore concentrate and magnetic separation tailings, wherein the mass of the obtained iron ore concentrate is 748.3 g.
XRD analysis of the obtained sulfur and iron ore concentrate showed that the phase of the sulfur was mainly S as shown in FIGS. 4 and 56The obtained iron concentrate mineral phase is mainly ferroferric oxide. And sampling and detecting the purity of the sulfur and the iron content (reduced to ferroferric oxide) in the iron ore concentrate, wherein the purity of the sulfur reaches 93.3 percent, and the content of the ferroferric oxide in the iron ore concentrate reaches 87.1 percent. Sampling and analyzing SiO of magnetic separation tailings2The content is 89.5%, and the product can be used as adjuvant for building materials.
Comparative example 1:
the method of this comparative example for treating iron-containing tailings and pyrite was as follows:
(1) putting 1000g of iron-containing tailings # 1 into a tubular furnace, and slowly introducing nitrogen into the furnace (the introduction amount of the nitrogen is 3 times of the volume of a hearth) to exhaust air in the furnace; starting heating, continuously introducing nitrogen at the speed of 100mL/min, heating to 800 ℃, keeping the temperature for roasting for 1.5h, stopping introducing nitrogen after the temperature of the tubular furnace is reduced to 50 ℃ after roasting is finished, taking out roasted slag, grinding until the fineness is-0.075 mm and accounts for about 85%, and then carrying out magnetic separation, wherein the strength for magnetic separation is 150 kA.m-1The results show that only 7.5g of iron concentrate is obtained.
(2) Placing 135g of pyrite into a tube furnace, and slowly introducing nitrogen into the furnace (the introduction amount of the nitrogen is 3 times of the volume of a hearth) to exhaust air in the furnace; opening the roasting furnace for heating, continuously introducing nitrogen at the speed of 100mL/min, raising the temperature to 800 ℃, keeping the temperature for roasting for 1.5h, discharging gas in the roasting process, and cooling to ensure that the gas is inSeparating out 13g of sulfur, pumping cooling gas to an inert gas vent hole and introducing the inert gas vent hole into the furnace to realize recycling, stopping introducing nitrogen after the temperature of the tubular furnace is reduced to 50 ℃ after the roasting, taking out the roasted slag, grinding the roasted slag until the fineness is-0.075 mm and the ore accounts for 85 percent, and performing magnetic separation, wherein the strength used for the magnetic separation is 150 kA.m-1And obtaining iron ore concentrate and magnetic separation tailings, wherein the mass of the iron ore concentrate is only 2.7 g.
Example 2:
the invention discloses a method for preparing iron ore concentrate and sulfur by the synergistic treatment of iron-containing tailings and pyrite, which comprises the following steps:
(1) 1000g of iron-containing tailings # 1 and 135g of pyrite (molar ratio Fe)2O3:FeS21:0.25)) and uniformly mixing to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a tubular furnace, slowly introducing nitrogen with the volume 3 times that of a hearth to exhaust air in the furnace, starting a heating device of a roasting furnace, continuously introducing nitrogen at the rate of 100mL/min, raising the temperature to 1000 ℃, keeping the temperature, roasting for 1.5h, discharging flue gas in the roasting process, cooling to separate out sulfur in the gas to obtain 64g of sulfur, and pumping cooling gas to an inert gas vent hole and introducing the gas into the furnace to realize recycling;
(3) after the temperature of the tubular furnace is reduced to 50 ℃, stopping introducing nitrogen, taking out the roasted slag, grinding the roasted slag until the fineness is minus 0.075mm and accounts for 90 percent, and then carrying out magnetic separation, wherein the intensity for the magnetic separation is 120 kA.m-1And obtaining iron ore concentrate and magnetic separation tailings, wherein the mass of the obtained iron ore concentrate is 727.0 g.
Sampling and detecting the purity of the sulfur and the iron content (reduced to ferroferric oxide) in the iron ore concentrate, wherein the purity of the sulfur reaches 95.7 percent, and the content of the ferroferric oxide in the iron ore concentrate reaches 81.6 percent.
Example 3:
a method for preparing iron ore concentrate and sulfur by the synergistic treatment of iron-containing tailings and pyrite comprises the following steps:
(1) 1000g of iron-containing tailings # 1 and 230g of pyrite (molar ratio Fe)2O3:FeS21:0.5) grinding and uniformly mixing to obtain a mixture;
(2) Putting the mixture obtained in the step (1) into a tubular furnace, slowly introducing nitrogen with the volume being 1 time of that of a hearth to completely exhaust air in the furnace, starting a heating device, continuously introducing nitrogen at the rate of 40mL/min, raising the temperature to 700 ℃, keeping the temperature, roasting for 1.5h, discharging gas in the roasting process, cooling to separate out sulfur in the gas to obtain 87g of sulfur, and pumping cooling gas to an inert gas vent hole to be introduced into the furnace to realize recycling;
(3) after the temperature of the tubular furnace is reduced to 50 ℃, stopping introducing nitrogen, taking out the roasted slag, grinding the roasted slag until the fineness is-0.075 mm and the content of 85 percent, and performing magnetic separation, wherein the strength for the magnetic separation is 180 kA.m-1Wherein the mass of the obtained iron ore concentrate is 610.6 g.
Sampling and detecting the purity of the sulfur and the iron content (reduced to ferroferric oxide) in the iron ore concentrate, wherein the purity of the sulfur reaches 97.4 percent, and the content of the ferroferric oxide in the iron ore concentrate reaches 78.4 percent.
Example 4:
the invention discloses a method for preparing iron ore concentrate and sulfur by the synergistic treatment of iron-containing tailings and pyrite, which comprises the following steps:
(1) 1000g of iron-containing tailings # 2 and 111g of pyrite (molar ratio Fe)2O3:FeS21:0.3) grinding and uniformly mixing to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a tubular furnace, slowly introducing inert gas argon gas with the volume being 1 time of that of a hearth to completely exhaust air in the furnace, starting a heating device, continuously introducing the inert gas argon gas at the speed of 50mL/min, raising the temperature to 900 ℃, carrying out heat preservation roasting for 1.5h, discharging gas in the roasting process, cooling to separate out sulfur in the gas to obtain 40.9g of sulfur, and pumping cooling gas to an inert gas vent hole and introducing the gas into the furnace to realize recycling;
(3) after the temperature of the tubular furnace is reduced to 50 ℃, stopping introducing nitrogen, taking out the roasted slag, grinding the roasted slag until the fineness is-0.075 mm and the content of 90 percent, and performing magnetic separation, wherein the strength used for the magnetic separation is 130 kA.m-1And obtaining iron ore concentrate and magnetic separation tailings, wherein the mass of the obtained iron ore concentrate is 513.7 g.
Sampling and detecting the purity of the sulfur and the iron content (reduced to ferroferric oxide) in the iron ore concentrate, wherein the purity of the sulfur reaches 87.5 percent, and the content of the ferroferric oxide in the iron ore concentrate reaches 90.1 percent.
Claims (9)
1. A method for preparing iron ore concentrate and sulfur by the synergistic treatment of iron-containing tailings and pyrite is characterized by comprising the following steps:
(1) mixing the iron-containing tailings with pyrite;
(2) carrying out high-temperature roasting treatment on the mixture obtained in the step (1) under the protection of inert gas, cooling gas generated by high-temperature roasting, and cooling to obtain a solid product, namely sulfur;
(3) and (3) carrying out magnetic separation on the roasting slag obtained by roasting in the step (2) to obtain iron ore concentrate and magnetic separation tailings.
2. The method according to claim 1, wherein in the step (1), the iron-containing tailings and the pyrite are added in an amount of 0.2 to 0.5 mol per mol of iron trioxide based on the iron trioxide in the iron-containing tailings and the iron disulfide in the pyrite.
3. The method of claim 1, wherein in the step (2), the high-temperature roasting temperature is 500-1000 ℃, and the high-temperature roasting time is not less than 20 min.
4. The method of claim 1, wherein in step (2), the cooled gas is recycled.
5. The method of claim 1, wherein in the step (2), before the high-temperature roasting treatment, an inert gas is introduced into the roasting furnace, and air is exhausted to form an inert atmosphere in the furnace.
6. The method according to any one of claims 1 to 5, wherein in the step (2), the inert gas is continuously introduced into the reaction furnace during the high-temperature roasting treatment at a rate of not less than 10 mL/min.
7. The method according to any one of claims 1 to 5, wherein in the step (3), the calcine slag is subjected to ore grinding treatment before magnetic separation, and the ore grinding particle size is-0.075 mm and accounts for 85-90%.
8. The method according to any one of claims 1 to 5, wherein in the step (3), the magnetic field intensity for magnetic separation is 100 to 200 kA-m-1。
9. The method of any one of claims 1 to 5, wherein the iron-containing tailings are mainly from smelting tailings of a smelting enterprise, and the main iron-containing component is Fe2O3。
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1205304A (en) * | 1997-07-11 | 1999-01-20 | 鲜荣忠 | Smelting sulphur by blocking fined sulphur ore powder and flume sand containing sulphur |
CN101570341A (en) * | 2009-05-26 | 2009-11-04 | 华中科技大学 | Method for utilizing comprehensive resource of sulfur-containing solid waste |
CN101585513A (en) * | 2009-06-11 | 2009-11-25 | 周超 | Method for roasting pyrite in sulfuric acid production |
CN102206743A (en) * | 2011-04-20 | 2011-10-05 | 北京化工大学 | Method for processing red mud by utilizing iron pyrites |
CN102320761A (en) * | 2011-06-03 | 2012-01-18 | 云南常青树投资有限公司 | Method for preparing cement active mixed material and concrete active admixture |
CN105084323A (en) * | 2015-09-15 | 2015-11-25 | 刘慧南 | System and method for manufacturing sulfur and iron oxide by using pyrite |
CN206986244U (en) * | 2017-06-15 | 2018-02-09 | 江苏省冶金设计院有限公司 | The system for handling troilite concentrate |
-
2020
- 2020-10-29 CN CN202011179111.5A patent/CN112458276A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1205304A (en) * | 1997-07-11 | 1999-01-20 | 鲜荣忠 | Smelting sulphur by blocking fined sulphur ore powder and flume sand containing sulphur |
CN101570341A (en) * | 2009-05-26 | 2009-11-04 | 华中科技大学 | Method for utilizing comprehensive resource of sulfur-containing solid waste |
CN101585513A (en) * | 2009-06-11 | 2009-11-25 | 周超 | Method for roasting pyrite in sulfuric acid production |
CN102206743A (en) * | 2011-04-20 | 2011-10-05 | 北京化工大学 | Method for processing red mud by utilizing iron pyrites |
CN102320761A (en) * | 2011-06-03 | 2012-01-18 | 云南常青树投资有限公司 | Method for preparing cement active mixed material and concrete active admixture |
CN105084323A (en) * | 2015-09-15 | 2015-11-25 | 刘慧南 | System and method for manufacturing sulfur and iron oxide by using pyrite |
CN206986244U (en) * | 2017-06-15 | 2018-02-09 | 江苏省冶金设计院有限公司 | The system for handling troilite concentrate |
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