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CN115747400B - 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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CN115747400B
CN115747400B CN202211502798.0A CN202211502798A CN115747400B CN 115747400 B CN115747400 B CN 115747400B CN 202211502798 A CN202211502798 A CN 202211502798A CN 115747400 B CN115747400 B CN 115747400B
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CN115747400A (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 iron concentrate, which comprises the steps of heating the iron concentrate by microwaves and then cooling to obtain a reduced material;sequentially grinding the reduction materials, removing impurities, and drying to obtain high-end sponge iron powder; the iron concentrate powder has total iron content of 60-71% and SiO 2 The content is 2-17%, O 2 The content is 22-27%, and the granularity is-200 mesh. The invention adopts microwave clean heating reducing gas as reducing agent, so that the direct reduction temperature is 100-200 ℃ lower than the traditional direct reduction temperature, the whole process has no carbon emission, 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 of 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 fine iron powder.
Background
The iron fine powder is ferroferric oxide powder with the total iron content of 60-71% and granularity of-200 meshes after the magnetite ore of Shanxi Jianshan and Fenugreek mountain is carefully selected and purified by ball milling magnetic separation equipment. The cleanliness of the iron concentrate powder is very rare in China or even worldwide, the iron powder is clean iron powder, most of the iron powder is used as stainless steel raw materials by Shanxi Taisteel, taisteel stainless steel can be known worldwide, the clean iron concentrate powder is also the biggest reason except for technical reasons, the technology of directly reducing (including secondary reduction) iron powder to produce sponge iron generally adopts coal-based traditional heating to produce primary reduced iron powder, and then gas-based secondary reduction is carried out to remove carbon. The high-quality clean high-end sponge iron powder in China mainly depends on import and is high in price, the high-value utilization of the high-quality fine iron powder is imperative, and the high-value utilization of the fine iron powder of Shanxi mountain fox and Gushan mountain has great significance for the field of high-end iron production in China.
Disclosure of Invention
The invention aims to provide a method for producing high-end sponge iron powder from fine iron powder, which uses microwaves to heat reducing gas to reduce the iron powder, uses protective gas to cool, grinds and adds medium water, removes impurities, dries tail gas to obtain high-quality sponge iron with total iron content of more than 99%, metallization rate of more than 99.9% and less harmful impurity content, reduces energy loss and gas loss, improves heat energy utilization rate, and improves production efficiency.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for producing high-end sponge iron powder from fine iron powder, which is characterized by comprising the following steps:
sequentially heating and cooling the iron concentrate by microwaves to obtain a reduced material;
grinding the reduction materials in sequence, removing impurities, and drying to obtain high-end sponge iron powder;
the iron concentrate powder has total iron content of 60-71% and SiO 2 The content is 2-17%, 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 temperature of the microwave heating 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 is composed of hydrogen.
Preferably, the cooling mode is to introduce protective gas 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 materials obtained after grinding is-800 meshes.
Preferably, the particle size of the material is more than 80% of the particle size of-1250 mesh.
Preferably, the impurity removal is magnetic separation impurity removal, and the magnetic field strength 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 has a total iron content of more than 99%, a metallization rate of more than 99.9%, a silicon dioxide content of less than 0.03%, and zero sulfur, phosphorus, arsenic, antimony and bismuth harmful substances
The beneficial technical effects of the invention are as follows:
the invention provides a method for producing high-end sponge iron powder from iron fine powder. The invention uses the characteristic of strong wave absorption of ferroferric oxide under microwave irradiation to reduce the materials by self-heating, the total power of the microwave is only 30KW, the total iron content of the produced high-end sponge iron powder is more than 99.6%, the metallization rate is more than 99%, the steelmaking harmful substances such as sulfur, phosphorus, arsenic, antimony, bismuth and the like are zero, the silicon dioxide is less than 0.03%, and the granularity of-800 meshes is 80% of the total pass-1250 meshes, thus belonging to clean high-quality high-end sponge iron powder.
Drawings
Fig. 1 is a process flow diagram of the production of 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 heating and cooling the iron concentrate by microwaves to obtain a reduced material;
grinding the reduction materials in sequence, removing impurities, and drying to obtain high-end sponge iron powder;
the iron concentrate powder has total iron content of 60-80%, granularity of-200 mesh and other elements less than 0.1%.
And heating the iron concentrate by microwaves and then cooling to obtain a reduced material.
The invention sequentially heats and cools the iron concentrate by microwaves to obtain a reduction material.
In the invention, the main components and the content of the iron concentrate are preferably as follows: TFe60-71%, siO 2 2-17%,O 2 22-27%, more preferably 65-70% TFe, siO 2 4-10%,O 2 24-26%, most preferably TFe66%, siO 2 8.7%,O 2 25.2%; the mesh number of the iron concentrate powder is-200 meshes, wherein-300 meshes account for 40%.
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 to 2 hours, more preferably 1.5 hours; 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 reducing atmosphere is preferably introduced in an amount of 100 to 120 kg/h, more preferably 110 kg/h.
The iron concentrate powder is preferably loaded into a microwave high-temperature special box and then is sent into an industrial multimode microwave box-type kiln for reduction. In the invention, the iron concentrate is preferably loosely spread and paved into a microwave high-temperature special box, and the thickness of the iron concentrate is 20-30 cm.
The invention uses hydrogen as reducing agent, uses the strong wave-absorbing property of ferroferric oxide under microwave irradiation to self-heat and reduce the material, the total microwave power is only 30KW, the direct reduction temperature is 100-200 degree lower than the traditional direct reduction temperature, no carbon emission is generated in the whole process, the product has no carburization phenomenon, the quality is superior and stable, and the energy consumption is low.
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 oxygen-proof cooling by introducing a protective gas, and the protective gas is preferably nitrogen, helium, neon or argon, and more preferably nitrogen.
The special microwave heating box after microwave heating is preferably pulled into the shielding gas cooling section through the box pulling machine to perform anaerobic cooling. According to the invention, the reduced material is prevented from being oxidized by anaerobic cooling.
After the reducing material is obtained, the reducing material is sequentially ground, decontaminated and dried to obtain the high-end sponge iron powder.
In the present invention, the time of the grinding is preferably 20 to 40min, more preferably 30min; the particle size of the material obtained after grinding is preferably-800 meshes, more preferably-1250 meshes accounting for more than 80 percent. The grinding is preferably wet grinding after mixing the reducing material with water; the mass of the water is preferably 2-4 times, more preferably 3 times, the mass of the reduced material; the water is preferably magnetic separation wastewater.
In the invention, the impurity removal is preferably magnetic separation 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 70-90 ℃, more preferably 80 ℃.
The invention preferably dehydrates the materials obtained after impurity removal under the protection gas before drying.
The drying method uses the tail gas (high-temperature nitrogen and the like) cooled by the anaerobic cooling, the protective gas cooled by the anaerobic cooling is recycled, the three wastes are not discharged, and the method 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 content of total iron in the high-end sponge iron powder is more than 99%, the metallization rate is more than 99.9%, the content of silicon dioxide is less than 0.03%, and the iron recovery rate is more than 98%.
Example 1
1) TFe content was 66%, siO 2 The content is 8.78%, O 2 3 tons of mountain western fox, girl and mountain iron fine powder with the content of 25.2 percent are bulk-loaded into a microwave high-temperature special box with the specification: long x wide x high = 2.5M x 1.3 x 0.5M, layer thickness 0.3M.
2) And (3) conveying the loaded material box into an industrial multimode microwave box type kiln through a box pulling machine, closing a material inlet furnace door, and then introducing hydrogen to clean the air in the kiln through an exhaust valve to form a reducing atmosphere.
3) Starting a microwave emitter to emit microwaves, setting the microwave frequency to be 2.45GHz, setting the total power to be 30KW, continuously supplementing and reducing hydrogen, keeping micro-positive pressure in the furnace, avoiding air from entering, simultaneously keeping excessive hydrogen to be directly reduced, and when the temperature rises to 950 ℃ after 8 minutes, automatically adjusting the microwave radiation power to be 15KW, setting the frequency to be 2.45GHz, carrying out constant-temperature reduction for 45 minutes, then automatically closing the microwave emitter, and stopping emitting microwaves.
4) And automatically lifting the high-temperature resistant isolation furnace door of the cooling section and the reduction section, pulling the charging box into the nitrogen cooling section through the box pulling machine, placing the isolation door, performing anaerobic cooling on the material, and discharging the material to the nitrogen protection feeder under the protection of nitrogen by using the strong magnetic chuck unloader after the material is cooled to 70 ℃.
5) The materials are sent to a horizontal overflow forging mill for size mixing and grinding through a nitrogen protection feeder, medium water with the mass 3 times of the materials is added, and grinding is carried out for 20 minutes, so that the granularity of the product, namely-800 meshes, is fully passed, and the granularity of the product, namely-1250 meshes, is 80 percent.
6) The overflow ore pulp automatically flows into a semi-countercurrent magnetic separator to carry out one-time weak magnetic separation, the magnetic field strength is 80MT, and the iron powder ore pulp after magnetic separation flows into a ceramic disc filter to be dehydrated under the protection of nitrogen.
7) The dehydrated high-end sponge iron powder is sent to a cooling tail gas three-cylinder dryer through a nitrogen protection feeder, and the high-end sponge iron powder is dried at 80 ℃.
8) And (3) conveying the obtained high-end sponge iron powder to a nitrogen hopper for vacuum bagging, and enabling the magnetic separation wastewater to flow into a reservoir through a pipeline for clarification to be used as slurry mixing water of a ball mill.
And (3) taking the obtained high-end sponge iron powder for delivery and identification mechanism, wherein the high-end sponge iron powder is detected to have the total iron content of 99.7%, the metallization rate of 99.9%, the silicon dioxide content of 0.01%, the iron recovery rate of 98.2%, the sulfur, phosphorus, arsenic, antimony and bismuth harmful substances of zero, and the granularity of-800 meshes of the high-end sponge iron powder is 80% of that of-1250 meshes.
Example 2
1) TFe content was 60%, siO 2 The content is 17.13%, O 2 The special box for microwave high temperature is filled with 3 tons of fine powder of mountain western fox, girl and mountain iron with the content of 22.87 percent in bulk, and the specification of the box is as follows: long x wide x high = 2.5M x 1.3 x 0.5M, layer thickness 0.3M.
2) And (3) conveying the loaded material box into an industrial multimode microwave box type kiln through a box pulling machine, closing a material inlet furnace door, and then introducing hydrogen to clean the air in the kiln through an exhaust valve to form a reducing atmosphere.
3) Starting a microwave emitter to emit microwaves, setting the microwave frequency to be 2.45GHz, setting the total power to be 25KW, continuously supplementing and reducing hydrogen, keeping micro-positive pressure in the furnace, avoiding air from entering, simultaneously keeping excessive hydrogen to be directly reduced, and when the temperature rises to 800 ℃ after 8 minutes, automatically adjusting the microwave radiation power to be 15KW and the frequency to be 2.45GHz by a control system, performing constant-temperature reduction for 30 minutes, and then automatically closing the microwave emitter to stop emitting microwaves.
4) And automatically lifting the high-temperature resistant isolation furnace door of the cooling section and the reduction section, pulling the charging box into the helium cooling section through the box pulling machine, putting down the isolation door, performing anaerobic cooling on the material, and unloading the material into an inert gas protection feeder under the protection of helium by using a strong magnetic chuck unloader after the material is cooled to 60 ℃.
5) The materials are sent to a horizontal overflow forging mill for size mixing and grinding through an inert gas protection feeder, medium water with the mass 2 times of the materials is added, and grinding is carried out for 30 minutes, so that the granularity of the product, namely-800 meshes, is completely through, and the granularity of the product, namely-1250 meshes, is 70 percent.
6) The overflow ore pulp automatically flows into a semi-countercurrent magnetic separator to carry out one-time weak magnetic separation, the magnetic field strength is 70MT, and the iron powder ore pulp after magnetic separation flows into a ceramic disc filter to be dehydrated under the protection of helium.
7) The dehydrated high-end sponge iron powder is sent to a cooling tail gas three-cylinder dryer through a nitrogen protection feeder, and the high-end sponge iron powder is dried at 90 ℃.
8) And (3) conveying the obtained high-end sponge iron powder to a nitrogen hopper for vacuum bagging, and enabling the magnetic separation wastewater to flow into a reservoir through a pipeline for clarification to be used as slurry mixing water of a ball mill.
And (3) taking the obtained high-end sponge iron powder for delivery and identification mechanism, wherein the high-end sponge iron powder is detected to have the total iron content of 99.3%, the metallization rate of 99.9%, the silicon dioxide content of 0.02%, the iron recovery rate of 97.3%, the sulfur, phosphorus, arsenic, antimony and bismuth harmful substances of zero, and the granularity of-800 meshes of 70% of the total pass-1250 meshes.
Example 3
1) TFe content was 68.9%, siO 2 The content is 4.83%, O 2 The special box for microwave high temperature is filled with 3 tons of fine powder of mountain fox, girl and mountain iron with the content of 26.3 percent in bulk, and the specification of the box is as follows: long x wide x high = 2.5M x 1.3 x 0.5M, layer thickness 0.3M.
2) And (3) conveying the loaded material box into an industrial multimode microwave box type kiln through a box pulling machine, closing a material inlet furnace door, and then introducing hydrogen to clean the air in the kiln through an exhaust valve to form a reducing atmosphere.
3) Starting a microwave emitter to emit microwaves, setting the microwave frequency to be 2.45GHz, setting the total power to be 35KW, continuously supplementing and reducing hydrogen, keeping micro-positive pressure in the furnace, avoiding air from entering, simultaneously keeping excessive hydrogen to be directly reduced, automatically adjusting the microwave radiation power to be 15KW by a control system when the temperature rises to 900 ℃ after 8 minutes, performing constant-temperature reduction at the frequency of 2.45GHz for 120 minutes, and then automatically closing the microwave emitter to stop emitting microwaves.
4) And automatically lifting the high-temperature resistant isolation furnace door of the cooling section and the reduction section, pulling the charging box into the argon cooling section through the box pulling machine, placing the isolation door, performing anaerobic cooling on the material, cooling the material to 80 ℃, and then discharging the material into an argon protection feeder under the protection of argon by using a strong magnetic chuck unloader.
5) The materials are sent to a horizontal overflow forging mill for size mixing and grinding through an argon protection feeder, medium water with the mass 4 times of the materials is added, and grinding is carried out for 40 minutes, so that the granularity of the product, namely-800 meshes, is completely through, and the granularity of the product, namely-1250 meshes, is 90 percent.
6) The overflow ore pulp automatically flows into a semi-countercurrent magnetic separator to carry out one-time weak magnetic separation, the magnetic field strength is 90MT, and the iron powder ore pulp after magnetic separation flows into a ceramic disc filter to be dehydrated under the protection of argon.
7) The dehydrated high-end sponge iron powder is sent to a cooling tail gas three-cylinder dryer through an argon protection feeder, and the high-end sponge iron powder is dried at 70 ℃.
8) And (3) conveying the low-temperature dried high-end sponge iron powder to an argon hopper for vacuum bagging, and enabling the magnetic separation wastewater to flow into a reservoir through a pipeline for clarification to be used as slurry mixing water of a ball mill.
And (3) taking the obtained high-end sponge iron powder for delivery and identification mechanism, wherein the high-end sponge iron powder is detected to have the total iron content of 99.6%, the metallization rate of 99.9%, the silicon dioxide content of 0.03%, the iron recovery rate of 98.6%, the sulfur, phosphorus, arsenic, antimony and bismuth harmful substances of zero, and the granularity of-800 meshes is 90% of the total pass-1250 meshes.

Claims (5)

1. A method for producing high-end sponge iron powder from fine iron powder, which is characterized by comprising the following steps:
sequentially heating and cooling the iron concentrate by microwaves to obtain a reduced material;
grinding the reduction materials in sequence, removing impurities, and drying to obtain high-end sponge iron powder;
the iron concentrate powder has total iron content of 60-71% and SiO 2 The content is 2-17%, O 2 The content is 22-27%, the granularity is-200 meshes, and other elements are less than 0.1%;
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 is composed of hydrogen;
the grinding time is 20-40min, and the granularity of the materials obtained after grinding is-800 meshes;
the granularity of the material is more than 80% of the granularity of-1250 meshes;
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 sulfur, phosphorus, arsenic, antimony and bismuth harmful substances of zero;
the microwave heating step comprises the following steps: firstly, the iron fine powder is put into a special microwave high-temperature box, and then is put into an industrial multimode microwave box-type kiln for reduction.
2. The method according to claim 1, wherein the cooling is performed by introducing a protective gas for anaerobic cooling; the protective gas is nitrogen, helium, neon or argon.
3. The method according to claim 1 or 2, wherein the temperature after cooling is 60-80 ℃.
4. The method of claim 1, wherein the removing of impurities is magnetic separation, and the magnetic field strength of the magnetic separation is 70-90MT.
5. The method according to claim 1, wherein the drying mode is tail gas residual temperature drying, and the drying temperature is 70-90 ℃.
CN202211502798.0A 2022-11-28 2022-11-28 Method for producing high-end sponge iron powder from fine iron powder Active CN115747400B (en)

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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 substances
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 substances
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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