CN115747400A - Method for producing high-end sponge iron powder from fine iron powder - Google Patents

Method for producing high-end sponge iron powder from fine iron powder Download PDF

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CN115747400A
CN115747400A CN202211502798.0A CN202211502798A CN115747400A CN 115747400 A CN115747400 A CN 115747400A CN 202211502798 A CN202211502798 A CN 202211502798A CN 115747400 A CN115747400 A CN 115747400A
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iron powder
content
end sponge
cooling
sponge iron
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CN115747400B (en
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李扬
李玉杰
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Abstract

The invention provides a method for producing high-end sponge iron powder from fine iron powder, which comprises the steps of heating the fine iron powder by microwave and then cooling the heated fine iron powder to obtain a reduced material; grinding the reduced materials in sequence, removing impurities, and drying to obtain high-end sponge iron powder; the total iron content of the used iron concentrate powder is 60-71%, and SiO is 2 2-17% of O 2 The content is 22-27%, and the granularity is-200 meshes. The invention adopts microwave clean heating reducing gas as a reducing agent, so that the direct reduction temperature is 100-200 ℃ lower than the traditional direct reduction temperature, no carbon emission exists in the whole process, the product has no carburization phenomenon, the quality is superior and stable, the total iron content is more than 99%, the metallization rate is more than 99.9%, the content of harmful impurities is less, and the energy consumption in the whole process is low.

Description

Method for producing high-end sponge iron powder from fine iron powder
Technical Field
The invention belongs to the field of clean smelting and utilization of iron powder, and particularly relates to a method for producing high-end sponge iron powder from refined iron powder.
Background
The iron concentrate powder is ferroferric oxide powder with a total iron content of 60-71% and a granularity of-200 meshes, wherein the ferroferric oxide powder is obtained by selecting and removing impurities from Jianshan in Shanxi and Nibea fox magnetite ores through ball milling magnetic separation equipment. The cleanliness of the fine iron powder is quite rare in the whole country and even the whole world, the fine iron powder belongs to clean iron powder, most of the iron powder is used as a stainless steel raw material by Shanxi Tai Steel, tai Steel stainless steel can be famous for the whole world, and the clean fine iron powder is the largest reason except for technical reasons. The high-quality clean high-end sponge iron powder in China mainly depends on import and is high in price, high-value utilization of the high-quality iron powder is imperative, and high-value utilization of the high-quality iron powder from Shanxi Jianzuo mountain is of great significance to the high-end iron production field in China.
Disclosure of Invention
The invention aims to provide a method for producing high-end sponge iron powder from refined iron powder, which comprises the steps of reducing the iron powder by heating reducing gas with microwaves, cooling the reduced iron powder by using protective gas, grinding the reduced iron powder and adding medium water, removing impurities, drying tail gas to obtain high-quality sponge iron with the total iron content of more than 99 percent, the metallization rate of more than 99.9 percent, less harmful impurities, reducing energy loss and gas loss, improving the heat energy utilization rate and improving the production efficiency.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for producing high-end sponge iron powder from fine iron powder is characterized by comprising the following steps:
sequentially carrying out microwave heating and cooling on the fine iron powder to obtain a reduced material;
grinding, removing impurities and drying the reduced materials in sequence to obtain high-end sponge iron powder;
the total iron content of the fine iron powder is 60-71%, and SiO is 2 2-17% of O 2 The content is 22-27%, the granularity is-200 meshes, and other elements are less than 0.1%.
Preferably, the microwave heating is performed in a reducing atmosphere.
Preferably, the microwave heating temperature is 800-950 ℃, the heating time is 0.5-2h, the microwave frequency is 2.45GHz, and the total input power is 25-35KW; the reducing atmosphere consists of hydrogen.
Preferably, the cooling mode is that protective gas is introduced for anaerobic cooling; the protective gas is nitrogen, helium, neon or argon.
Preferably, the temperature after cooling is 60-80 ℃.
Preferably, the grinding time is 20-40min, and the granularity of the material obtained after grinding is-800 meshes.
Preferably, the granularity of the material is-1250 meshes and accounts for more than 80 percent.
Preferably, the impurity removal is magnetic separation impurity removal, and the magnetic field intensity of the magnetic separation impurity removal is 70-90MT.
Preferably, the drying mode is tail gas residual temperature drying, and the drying temperature is 70-90 ℃.
Preferably, the high-end sponge iron powder is characterized in that the total iron content is more than 99%, the metallization rate is more than 99.9%, the silicon dioxide content is less than 0.03%, and harmful substances such as sulfur, phosphorus, arsenic, antimony and bismuth are zero
The invention has the beneficial technical effects that:
the invention provides a method for producing high-end sponge iron powder from refined iron powder. The invention utilizes the strong wave-absorbing property of ferroferric oxide under microwave irradiation to lead materials to be reduced by self-heating, the total power of microwave is only 30KW, the total iron of the produced high-end sponge iron powder is more than 99.6 percent, the metallization rate is more than 99 percent, the steelmaking harmful substances such as sulfur, phosphorus, arsenic, antimony, bismuth and the like are zero, the silicon dioxide is less than 0.03 percent, the granularity of-800 meshes is all through-1250 meshes accounting for 80 percent, and the invention belongs to clean high-quality high-end sponge iron powder.
Drawings
Fig. 1 is a process flow chart of producing high-end sponge iron powder from fine iron powder.
Detailed Description
The invention provides a method for producing high-end sponge iron powder from fine iron powder, which comprises the following steps:
sequentially carrying out microwave heating and cooling on the fine iron powder to obtain a reduced material;
sequentially grinding the reduced materials, removing impurities and drying to obtain high-end sponge iron powder;
the total iron content of the fine iron powder is 60-80%, the granularity is-200 meshes, and other elements are less than 0.1%.
And (3) heating the fine iron powder by microwave and then cooling to obtain a reduced material.
In the invention, the reduced material is obtained by sequentially heating and cooling the fine iron powder by microwave.
In the present invention, the main components and contents of the fine iron powder are preferably: TFe60-71%, siO 2 2-17%,O 2 22-27%, more preferably 65-70% of TFe, siO 2 4-10%,O 2 24-26%, most preferably 66% TFe, siO 2 8.7%,O 2 25.2 percent; the mesh number of the iron fine powder is-200 meshes, wherein-300 meshes account for 40 percent.
In the present invention, the microwave heating is preferably performed in a reducing atmosphere.
In the invention, the microwave heating temperature is preferably 800-1000 ℃, more preferably 850-950 ℃, and most preferably 900 ℃; the heating time is preferably 0.5-2h, more preferably 1.5h; the microwave frequency is preferably 2.45GHz; the total power is preferably 25-35KW, more preferably 30KW; the reducing atmosphere is preferably hydrogen, more preferably hydrogen; the introduction amount of the reducing atmosphere is preferably 100 to 120 kg/h, more preferably 110 kg/h.
The iron concentrate powder is preferably filled into a microwave high-temperature special box and then is conveyed into an industrial multi-mode microwave box type kiln for reduction. In the invention, the fine iron powder is preferably paved into a special microwave high-temperature box in a loose and flat manner, and the thickness of the fine iron powder is 20-30 cm.
The method takes hydrogen as a reducing agent, utilizes the characteristic of strong wave absorption of ferroferric oxide under microwave irradiation to lead the materials to be reduced by self-heating, and the total power of the microwave only needs 30KW to meet the requirement, thus leading the direct reduction temperature to be 100-200 ℃ lower than the price of the traditional direct reduction temperature, having no carbon emission in the whole process, having no carburization phenomenon, excellent and stable quality and low energy consumption.
In the present invention, the temperature after cooling is preferably 60 to 80 ℃, more preferably 65 to 75 ℃, and most preferably 70 ℃; the cooling mode is preferably anaerobic cooling by introducing protective gas, and the protective gas is preferably nitrogen, helium, neon or argon, and more preferably nitrogen.
The invention preferably pulls the microwave heating special box after microwave heating into the protective gas cooling section through the box pulling machine for anaerobic cooling. The reduced material is prevented from being oxidized by anaerobic cooling.
After the reduction material is obtained, the invention sequentially grinds, removes impurities and dries the reduction material to obtain the high-end sponge iron powder.
In the present invention, the time for the grinding is preferably 20 to 40min, more preferably 30min; the particle size of the material obtained after grinding is preferably-800 meshes, and more preferably-1250 meshes accounting for more than 80%. The grinding is preferably wet grinding after mixing the reduced material and water; the mass of the water is preferably 2-4 times, more preferably 3 times of that of the reduction material; the water is preferably magnetic separation waste water.
In the invention, the impurity removal is preferably magnetic impurity removal; the magnetic field strength is preferably 70-90MT, more preferably 80MT.
In the invention, the drying mode is preferably tail gas residual temperature drying; the temperature of the drying is preferably 70 to 90 ℃, more preferably 80 ℃.
The invention firstly dehydrates the materials obtained after impurity removal under the protection of gas before drying.
The invention dries the anoxybiotic cooled tail gas (high-temperature nitrogen and the like), and the anoxybiotic cooled protective gas is recycled, no three wastes are discharged, and the invention is environment-friendly and belongs to clean production.
The invention also provides the high-end sponge iron powder prepared by the preparation method, wherein the high-end sponge iron powder has the total iron content of more than 99%, the metallization rate of more than 99.9%, the silicon dioxide content of less than 0.03% and the iron recovery rate of more than 98%.
Example 1
1) The content of TFe is 66 percent and SiO is added 2 Content of 8.78%, O 2 3 tons of Shanxi Fox Nippon holly mountain iron fine powder with the content of 25.2 percent are loosely packed into a special microwave high-temperature box, and the specification of the box is as follows: length, width, height =2.5m, 1.3, 0.5m, and layer thickness 0.3M.
2) And (3) conveying the loaded material box into an industrial multi-mode microwave box type kiln through a box pulling machine, closing a material inlet furnace door, introducing hydrogen, and exhausting air in the kiln through an exhaust valve to form a reducing atmosphere.
3) Starting a microwave emitter to emit microwaves, setting the frequency of the microwaves to be 2.45GHz and the total power to be 30KW, continuously supplementing reduction hydrogen, keeping micro-positive pressure in the furnace, avoiding air from entering, simultaneously keeping excessive hydrogen to be directly reduced, leading the hydrogen into the furnace at a rate of 110 kg/h, automatically adjusting the microwave radiation power to be 15KW and the frequency to be 2.45GHz when the temperature rises to 950 ℃ after 8 minutes, carrying out constant-temperature reduction for 45 minutes, then automatically closing the microwave emitter, and stopping emitting the microwaves.
4) The high-temperature resistant isolation furnace door of the cooling section and the reduction section is automatically lifted, the charging box is pulled into the nitrogen cooling section through the box pulling machine to put down the isolation door, the material is subjected to anaerobic cooling, and the material is unloaded into the nitrogen protection feeder under the protection of nitrogen by using the strong magnetic chuck unloader after being cooled to 70 ℃.
5) The materials are conveyed to a horizontal overflow forging mill through a nitrogen protection feeder to be mixed and ground, medium water with the mass 3 times of that of the materials is added, and grinding is carried out for 20 minutes, so that the product with the granularity of-800 meshes completely passes through-1250 meshes and accounts for 80 percent.
6) And enabling the overflow ore pulp to automatically flow into a semi-countercurrent magnetic separator for primary weak magnetic separation, wherein the magnetic field intensity is 80MT, and the iron powder ore pulp after magnetic separation flows into a ceramic disc filter for dehydration under the protection of nitrogen.
7) And (4) conveying the dehydrated high-end sponge iron powder to a tail gas cooling three-cylinder dryer through a nitrogen protection feeder, and drying the high-end sponge iron powder at 80 ℃.
8) And conveying the obtained high-end sponge iron powder to a nitrogen hopper for vacuum bagging, and allowing the magnetic separation wastewater to flow into a reservoir through a pipeline for clarification to be used as water for ball mill size mixing.
The obtained high-end sponge iron powder is taken to be delivered to an identification mechanism, the detected total iron content of the high-end sponge iron powder is 99.7 percent, the metallization rate is 99.9 percent, the silicon dioxide content is 0.01 percent, the iron recovery rate is 98.2 percent, the sulfur, phosphorus, arsenic, antimony and bismuth are zero, and the particle size of-800 meshes of all-1250 meshes accounts for 80 percent.
Example 2
1) The TFe content is 60 percent and SiO is added 2 Content of 17.13%, O 2 3 tons of Shanxi Fox Nippon holly mountain iron fine powder with the content of 22.87 percent are loosely packed into a special microwave high-temperature box, and the specification of the box is as follows: length, width, height =2.5m 13 × 0.5m, layer thickness 0.3M.
2) And (3) conveying the loaded material box into an industrial multi-mode microwave box type kiln through a box pulling machine, closing a material inlet furnace door, introducing hydrogen, and exhausting air in the kiln through an exhaust valve to form a reducing atmosphere.
3) Starting a microwave emitter to emit microwaves, setting the frequency of the microwaves to be 2.45GHz, setting the total power to be 25KW, continuously supplementing reduction hydrogen, keeping the micro-positive pressure in the furnace, avoiding air from entering, simultaneously keeping excessive hydrogen to be directly reduced, setting the introduction amount of the hydrogen to be 100 kg/h, automatically adjusting the microwave radiation power to be 15KW by a control system when the temperature rises to 800 ℃ after 8 minutes, carrying out constant-temperature reduction at the frequency of 2.45GHz, keeping the constant-temperature time to be 30 minutes, then automatically closing the microwave emitter, and stopping emitting the microwaves.
4) And (3) automatically lifting a high-temperature-resistant isolation furnace door of the cooling section and the reduction section, pulling the charging box into the helium cooling section through a box pulling machine, putting down the isolation door, carrying out anaerobic cooling on the materials, and unloading the materials into an inert gas protection feeder under the protection of helium by using a strong magnetic chuck unloader after the materials are cooled to 60 ℃.
5) The materials are conveyed to a horizontal overflow forging mill through an inert gas protection feeder to be mixed and ground, medium water with the mass 2 times that of the materials is added, and grinding is carried out for 30 minutes, so that the product with the granularity of-800 meshes completely passes through-1250 meshes and accounts for 70 percent.
6) And enabling the overflow ore pulp to automatically flow into a semi-countercurrent magnetic separator for primary weak magnetic separation, enabling the magnetic field intensity to be 70MT, and enabling the iron powder ore pulp subjected to magnetic separation to flow into a ceramic disc filter for dehydration under the protection of helium.
7) And (4) conveying the dehydrated high-end sponge iron powder to a tail gas cooling three-cylinder dryer through a nitrogen protection feeder, and drying the high-end sponge iron powder at 90 ℃.
8) And conveying the obtained high-end sponge iron powder to a nitrogen hopper for vacuum bagging, and allowing the magnetic separation wastewater to flow into a reservoir through a pipeline for clarification to be used as water for ball mill size mixing.
The obtained high-end sponge iron powder is taken to be delivered to an identification mechanism, and the detected high-end sponge iron powder has the total iron content of 99.3 percent, the metallization rate of 99.9 percent, the silicon dioxide content of 0.02 percent, the iron recovery rate of 97.3 percent, zero harmful substances of sulfur, phosphorus, arsenic, antimony and bismuth, and 70 percent of particles with the particle size of-800 meshes which completely pass through-1250 meshes.
Example 3
1) The TFe content is 68.9 percent, siO 2 Content of 4.83%, O 2 3 tons of Shanxi Niuzu mountain iron fine powder with the content of 26.3 percent are loosely put into a special microwave high-temperature box, and the specification of the box is as follows: length, width, height =2.5m, 1.3, 0.5m, and layer thickness 0.3M.
2) And (3) conveying the loaded material box into an industrial multi-mode microwave box type kiln through a box pulling machine, closing a material inlet furnace door, introducing hydrogen, and exhausting air in the kiln through an exhaust valve to form a reducing atmosphere.
3) Starting a microwave emitter to emit microwaves, setting the frequency of the microwaves to be 2.45GHz and the total power to be 35KW, continuously supplementing reduction hydrogen, keeping micro-positive pressure in the furnace, avoiding air from entering, simultaneously keeping excessive hydrogen to be directly reduced, leading the hydrogen into the furnace at a rate of 120 kg/h, automatically adjusting the microwave radiation power to be 15KW and the frequency to be 2.45GHz when the temperature rises to 900 ℃ after 8 minutes, carrying out constant-temperature reduction for 120 minutes, then automatically closing the microwave emitter, and stopping emitting the microwaves.
4) The high-temperature resistant isolation furnace door of the cooling section and the reduction section is automatically lifted, the charging box is pulled into the argon cooling section through the box pulling machine to put down the isolation door, the material is subjected to anaerobic cooling, and the material is unloaded into the argon protection feeder under the protection of argon by utilizing the strong magnetic chuck unloader after being cooled to 80 ℃.
5) The material is sent to a horizontal overflow forging mill for size mixing and grinding through an argon protection feeder, medium water with the mass 4 times that of the material is added, and grinding is carried out for 40 minutes, so that the product with the granularity of-800 meshes completely passes through-1250 meshes and accounts for 90 percent.
6) And enabling the overflow ore pulp to automatically flow into a semi-countercurrent magnetic separator for primary weak magnetic separation, wherein the magnetic field intensity is 90MT, and the iron powder ore pulp after magnetic separation flows into a ceramic disc type filter for dehydration under the protection of argon.
7) And (4) conveying the dehydrated high-end sponge iron powder to a tail gas cooling three-cylinder dryer through an argon protection feeder, and drying the high-end sponge iron powder at 70 ℃.
8) And drying the high-end sponge iron powder at low temperature, conveying the high-end sponge iron powder to an argon gas hopper for vacuum bagging, and allowing the magnetic separation wastewater to flow into a reservoir through a pipeline for clarification to be used as water for ball mill size mixing.
The obtained high-end sponge iron powder is taken to be delivered to an identification mechanism, the detected total iron content of the high-end sponge iron powder is 99.6 percent, the metallization rate is 99.9 percent, the silicon dioxide content is 0.03 percent, the iron recovery rate is 98.6 percent, the sulfur, phosphorus, arsenic, antimony and bismuth are zero, and the particle size of-800 meshes of all-1250 meshes accounts for 90 percent.

Claims (10)

1. A method for producing high-end sponge iron powder from fine iron powder is characterized by comprising the following steps:
sequentially carrying out microwave heating and cooling on the fine iron powder to obtain a reduced material;
grinding, removing impurities and drying the reduced materials in sequence to obtain high-end sponge iron powder;
the total iron content of the fine iron powder is 60-71%, and SiO is 2 2-17% of O 2 The content is 22-27%, the granularity is-200 meshes, and other elements are less than 0.1%.
2. The method of claim 1, wherein the microwave heating is performed in a reducing atmosphere.
3. The method according to claim 1 or 2, wherein the microwave heating temperature is 800-950 ℃, the heating time is 0.5-2h, the microwave frequency is 2.45GHz, and the total input power is 25-35KW; the reducing atmosphere consists of hydrogen.
4. The method according to claim 1, wherein the cooling mode is anaerobic cooling by introducing protective gas; the protective gas is nitrogen, helium, neon or argon.
5. The method according to claim 1 or 4, wherein the temperature after cooling is 60-80 ℃.
6. The preparation method according to claim 1, wherein the grinding time is 20-40min, and the particle size of the ground material is-800 meshes.
7. The method of claim 6, wherein the material has a particle size of 80% or more of-1250 mesh.
8. The method according to claim 1, wherein the impurity removal is magnetic impurity removal, and the magnetic field intensity of the magnetic impurity removal is 70-90MT.
9. The method according to claim 1, wherein the drying mode is tail gas waste heat drying, and the drying temperature is 70-90 ℃.
10. The high-end sponge iron powder prepared by the method of any one of claims 1 to 9, wherein the high-end sponge iron powder has a total iron content of more than 99%, a metallization rate of more than 99.9%, a silica content of less than 0.03%, and zero harmful substances such as sulfur, phosphorus, arsenic, antimony and bismuth.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010222667A (en) * 2009-03-25 2010-10-07 Nippon Steel Corp Method for reducing iron oxide-containing material
CN102839250A (en) * 2012-09-28 2012-12-26 昆明理工大学 Method for collecting high-quality coal gas in process of producing reduced iron powder by means of microwave heating
CN106238745A (en) * 2016-08-19 2016-12-21 朝阳金河粉末冶金材料有限公司 The method utilizing strip stove temperature production reduced iron powder
CN107034356A (en) * 2017-05-09 2017-08-11 江苏省冶金设计院有限公司 A kind of method of microwave tunnel kiln reduction apparatus and its smart iron ore of reduction
CN113462842A (en) * 2021-05-31 2021-10-01 钢研晟华科技股份有限公司 Method for preparing high-titanium slag powder and metal iron powder by reducing ilmenite concentrate powder at low temperature

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010222667A (en) * 2009-03-25 2010-10-07 Nippon Steel Corp Method for reducing iron oxide-containing material
CN102839250A (en) * 2012-09-28 2012-12-26 昆明理工大学 Method for collecting high-quality coal gas in process of producing reduced iron powder by means of microwave heating
CN106238745A (en) * 2016-08-19 2016-12-21 朝阳金河粉末冶金材料有限公司 The method utilizing strip stove temperature production reduced iron powder
CN107034356A (en) * 2017-05-09 2017-08-11 江苏省冶金设计院有限公司 A kind of method of microwave tunnel kiln reduction apparatus and its smart iron ore of reduction
CN113462842A (en) * 2021-05-31 2021-10-01 钢研晟华科技股份有限公司 Method for preparing high-titanium slag powder and metal iron powder by reducing ilmenite concentrate powder at low temperature

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