CN115780816A - Production process of superfine atomized iron powder for new energy battery - Google Patents

Production process of superfine atomized iron powder for new energy battery Download PDF

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CN115780816A
CN115780816A CN202211614971.6A CN202211614971A CN115780816A CN 115780816 A CN115780816 A CN 115780816A CN 202211614971 A CN202211614971 A CN 202211614971A CN 115780816 A CN115780816 A CN 115780816A
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powder
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iron powder
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CN115780816B (en
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孙岩
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Jean Kane Bazhou Metal Powder Co ltd
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Abstract

In order to overcome the defect that the existing production line can not achieve the effects of high fine powder content and obvious yield, the invention provides a production process of superfine atomized iron powder for a new energy battery, which comprises the following steps: adding one or two of scrap steel or pig iron into an electric arc furnace according to a proportion for smelting; impacting the smelted mixed solution into powder slurry through an atomization system; removing part of nonmagnetic impurities by a wet magnetic separator, then extracting water in the slurry by a vacuum filter, drying the powder by a drying furnace, and then cooling; sieving the dried powder by a sieving machine, removing nonmagnetic impurities by a dry magnetic separator to obtain superfine atomized iron powder, and packaging and delivering; the invention uses the atomization system to impact the smelted mixed liquid into particles with the diameter less than or equal to 100 microns, thereby ensuring that the product has even particle size distribution, can remove non-magnetic impurities, has higher fine powder content and has obvious product yield effect.

Description

Production process of superfine atomized iron powder for new energy battery
Technical Field
The invention relates to the technical field of new energy battery materials, in particular to a production process of superfine atomized iron powder for a new energy battery.
Background
With the development of new energy automobiles, lithium iron phosphate (LiFePO) is gradually increased 4 ) The requirement of the battery anode material is that the process time for preparing the iron phosphate by using a chemical method is long, and the granularity and the purity of the product are not easy to control.
The current new process is to prepare iron phosphate powder by taking pure iron powder and phosphoric acid as raw materials. Lithium iron phosphate of the molecular formula LiFePO 4 Also called lithium iron phosphate and lithium iron phosphorus, abbreviated as LFP, is a positive electrode material of a lithium ion battery. It contains no noble elements such as cobalt, etc., and has low raw material price and the content of phosphorus, lithium and iron existing in the earth's resourcesIs rich in nutrients. Compared with other anode materials, the lithium iron phosphate has the advantages of wide raw materials, stable supply, low cost and the like.
According to the data of high-power lithium batteries and the sales volume of new energy automobiles, the automobile scale is increased by 4 times in 2020-2025 years, the corresponding power lithium battery shipment volume is increased by 5 times, and the small power and energy storage increases by 2 times and 4 times respectively. The method is expected to correspond to 317.6, 439.9, 611.5, 842.5 and 1162.9 thousands of vehicles in 21-25 years, correspond to 195.1, 318.1, 509.6, 842.5 and 349.0GWH of total power battery output, correspond to 97.6, 159.0, 254.8, 421.3 and 674.5GWH of power lithium iron phosphate battery output, 12.5, 18.9, 28.9, 40.6 and 56.9GWH of low-power and consumption lithium iron phosphate battery output, 3.0, 5.5, 10.1, 18.6 and 34.2GWH of energy storage communication lithium iron phosphate battery output, and total lithium iron phosphate demand in 2021-2025 years is respectively 28.3, 45.9, 73.4, 120.1 and 191.4 million tons.
At present, the market of fuel automobiles is accelerated and slowed down, and electric automobiles develop rapidly. With the development of new energy automobiles, the demand on the anode material of the lithium iron phosphate battery is gradually increased, the process time for preparing the iron phosphate by using a chemical method is longer, and the granularity and the purity of the product are not easy to control. The current new process is to prepare iron phosphate powder by taking pure iron powder and phosphoric acid as raw materials. Therefore, the research process finds that the Mn content in the molten steel can be reduced to 0.08% at least in the research of the superfine atomized iron powder for the new energy battery; the Cr content can be reduced to 0.02 percent at the lowest, the Cu content can be reduced to 0.015 percent at the lowest, and the market demand is that the Mn content is less than or equal to 0.030 percent, the Cr content is less than or equal to 0.015 percent, and the Cu content is less than or equal to 0.003 percent; therefore, how to overcome the above technical problems and disadvantages is an important problem to be solved.
Disclosure of Invention
The invention provides a production process of superfine atomized iron powder for a new energy battery, aiming at the problem that the existing production line cannot achieve the purposes of high fine powder content and obvious yield.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a production process of superfine atomized iron powder for a new energy battery, which comprises the following steps:
step one, charging: one or two of scrap steel or pig iron are added into an electric arc furnace according to a proportion;
step two, smelting: smelting scrap steel or pig iron or a mixture thereof in an electric arc furnace by using electric energy and chemical energy, wherein the smelting time is 130-160 minutes, the tapping temperature is 1700-1800 ℃, and mixed molten metal is formed after smelting;
step three, water atomization: in the atomization system, the adopted nozzle is rotary, and the rotating speed is 300-500 r/min; the width of the nozzle ring seam is 0.3-0.5 mm; the water pressure of the atomization system is 15-20 MPa, and the water flow is 140-160 m 3 H; the atomization temperature is 1400-1800 ℃; at the 10 cm position of the front end of the nozzle, carbon dioxide gas is passed through the nozzle, the specific flow rate is 3-5L/min, and the smelted mixed liquid is impacted into particles with the diameter less than or equal to 100 micrometers by an atomization system, so that powder slurry is formed.
The nozzle of rotation type can make the spray area increase of water smoke, has improved the production efficiency of iron powder, has reduced manufacturing cost.
The nozzle cascade seam is wide too, and the particle diameter that can make water smoke is great, and the nozzle cascade seam is wide too narrow, can make water smoke blowout unsmooth. The invention combines the width of the nozzle ring and the water pressure and water flow of the atomizing system, so that the particle size and penetrating power of the atomized water are excellent, and the production is well satisfied.
Water pressure is big, and it is big to make the penetrating power, and water flow is big, and the ejection rate that can make steam is high, and water pressure and water flow in the certain limit combine, can make mixed liquid obtain the abundant impact of water smoke, form more fine and close granule.
The carbon dioxide of specific velocity of flow is passed through to the nozzle front end for carbon dioxide forms supercritical state, when carbon dioxide combines with the water smoke with specific velocity of flow, can make water smoke refine more and even, and further make the iron powder more easily dispersed into the particle size littleer, more homogeneous granule. The distance that carbon dioxide lets in the water smoke is too close, can have certain influence to the velocity of flow and the pressure of water smoke, if the distance is too far away, can not play fine dispersion effect to the water smoke again. The addition of the carbon dioxide supercritical reduces the water consumption, improves the production efficiency, reduces the production cost and saves the energy. On the other hand, free carbon dioxide is used, so that carbon neutralization is realized while the production cost is saved and the energy consumption is reduced.
Harmful gases generated during the production of iron powder can be absorbed by supercritical carbon dioxide. The supercritical carbon dioxide fluid is colorless, tasteless and nontoxic in a normal state, has no solvent residue after being separated from the extracted components, can effectively avoid the solvent toxicity residue under the traditional solvent extraction condition, simultaneously prevents the toxicity of the extraction process to human bodies and the pollution to the environment, and is a natural and environment-friendly extraction technology.
All the technological parameters of the rotary nozzle, the rotating speed, the circumferential seam width of the nozzle, the water pressure and the water flow of the atomizing system, the distance and the flow velocity of supercritical carbon dioxide entering the water atomizing system and the like of the whole water atomizing system are complete systems, all the technological parameters are mutually synergistic, and the optimal effect cannot be achieved by changing any parameter.
Step four, dehydration and drying: the atomized slurry passes through a wet magnetic separator to enable the slurry containing iron powder to be adsorbed on a magnetic roller, part of nonmagnetic impurities are removed through washing of water, then the moisture in the slurry is extracted through a vacuum filter to enable the moisture content of the rest powder to be lower than 13%, then the powder is dried through a drying furnace, and then the dried powder is cooled through a water-cooling trough to enable the temperature of detected iron powder to be not more than 100 ℃;
step five, sieving and magnetic separation: conveying the dried powder to a screening machine through a bucket elevator for screening, and removing nonmagnetic impurities from the screened powder through a dry magnetic separator to obtain superfine atomized iron powder;
step six, packaging and delivering: and packaging the obtained superfine atomized iron powder to ensure that the bag is not damaged and the label is put well.
Optionally, the purity of the pig iron in the first step is 99.990-99.997%.
Optionally, the ratio of scrap steel or/and pig iron in the first step is as follows: when the copper content of the superfine atomized iron powder is less than 0.006 percent, the content of scrap steel is 0 and the content of pig iron is 100 percent; when the copper content of the superfine atomized iron powder is required to be between 0.007 and 0.010 percent, the content of the scrap steel is 15 percent, and the content of the pig iron is 85 percent; when the copper content of the superfine atomized iron powder is required to be between 0.011 percent and 0.014 percent, the content of scrap steel is 50 percent, and the content of pig iron is 50 percent; when the copper content of the superfine atomized iron powder is required to be more than 0.015 percent, the content of scrap steel is 100 percent, and the content of pig iron is 0.
Optionally, the electric arc furnace used in the step one or the step two is a 15-ton electric arc furnace.
Optionally, carbon powder, fluorite and lime are also added in the smelting process in the second step.
Optionally, 20-40 kg of carbon powder, 150-220 kg of fluorite and 600-900 kg of lime are added according to parts by weight.
Optionally, in the third step, the diameter of the zirconium core of the atomization system is 16mm, and the angle of the nozzle is 11 °.
Optionally, the vacuum pressure of the vacuum filter in the fourth step is-0.02 to-0.08 Mpa, and the rotating speed of the vacuum filter is 150 to 300r/min.
Optionally, in the fourth step, the exhaust temperature of the drying furnace is required to be 130-150 ℃.
Optionally, the screening machine in the fifth step adopts a 100-mesh screen.
According to the production process of the superfine atomized iron powder for the new energy battery, provided by the invention, an atomization system has the following innovative technologies: the rotary nozzle can increase the spray area of the water mist, improve the production efficiency of the iron powder and reduce the production cost.
The nozzle cascade seam is wide too, and the particle diameter that can make water smoke is great, and the nozzle cascade seam is wide too narrowly, can make the water smoke blowout unsmooth. The invention combines the width of the nozzle ring and the water pressure and water flow of the atomizing system, so that the particle size and penetrating power of the atomized water are excellent, and the production is well met.
Water pressure is big, and it is big to make the penetrating power, and water flow is big, and the ejection rate that can make steam is high, and water pressure and water flow in the certain limit combine, can make mixed liquid obtain the abundant impact of water smoke, form more fine and close granule.
The carbon dioxide of specific velocity of flow is passed through to the nozzle front end for carbon dioxide forms supercritical state, when carbon dioxide combines with the water smoke with specific velocity of flow, can make water smoke refine more and even, and further make the iron powder more easily dispersed into the particle size littleer, more homogeneous granule. The distance that carbon dioxide lets in the water smoke is too close, can have certain influence to the velocity of flow and the pressure of water smoke, if the distance is too far away, can not play fine dispersion effect to the water smoke again. The supercritical carbon dioxide is added, so that the adopted water amount is reduced, the production efficiency is improved, the production cost is reduced, and the energy is saved. On the other hand, free carbon dioxide is used, so that carbon neutralization is realized while the production cost is saved and the energy consumption is reduced.
Harmful gases generated during the production of iron powder can be absorbed by supercritical carbon dioxide. The supercritical carbon dioxide fluid is colorless, tasteless and nontoxic in a normal state, has no solvent residue after being separated from the extracted components, can effectively avoid the solvent toxicity residue under the traditional solvent extraction condition, simultaneously prevents the toxicity of the extraction process to human bodies and the pollution to the environment, and is a natural and environment-friendly extraction technology.
All technological parameters of the whole water atomization system, such as the rotating nozzles, the rotating speed, the circumferential seam width of the nozzles, the water pressure and the water flow of the atomization system, the distance and the flow rate of supercritical carbon dioxide entering the water atomization system and the like are complete systems, all technological parameters are mutually synergistic, and the optimal effect cannot be achieved by changing any parameter.
The mixed liquid after smelting is impacted into particles with the diameter less than or equal to 100 microns through an atomization system, so that the particle size distribution of the product is uniform, the particle size below a 100-mesh sieve can reach 99.8%, meanwhile, through two steps of dehydration drying and sieving magnetic separation, nonmagnetic impurities are removed, the content of fine powder is higher, the product yield effect is obvious, and the production cost is lower; the production process is simple and convenient, easy to operate and high in practicability. The novel steel-making two-line device is improved and optimized, so that the pollution of impurities is avoided, the cleanliness of the product is ensured, the metal powder can be effectively subjected to centralized treatment and collection, the resources are effectively saved, the working efficiency is improved, and the service life of the device is prolonged.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Experimental procedures without specifying specific conditions in the examples below, generally according to conditions conventional in the art or as recommended by the manufacturer; the raw materials, reagents and the like used are those commercially available from conventional markets and the like unless otherwise specified. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
The invention provides a production process of superfine atomized iron powder for a new energy battery, which comprises the following steps:
step one, charging: one or two of scrap steel or pig iron are added into an electric arc furnace according to a proportion;
the electric arc furnace adopted by the invention is produced by a 15-ton electric arc furnace, and an oxygen blowing mode at a furnace door is adopted; at present, most of domestic steel mills produce 50-ton electric arc furnaces, and the circular oxygen blowing mode around the furnace bottom is adopted, so that the 15-ton electric arc furnace used by the invention greatly reduces the production cost compared with the 50-ton electric arc furnace.
The purity of the pig iron in the invention is 99.990-99.997%. Meanwhile, the proportion of the scrap steel or/and the pig iron is determined by the following factors, when the copper content of the superfine atomized iron powder to be produced is less than 0.006 percent, the content of the scrap steel is 0, and the content of the pig iron is 100 percent; when the copper content of the superfine atomized iron powder is 0.007-0.010%, the content of scrap steel is 15%, and the content of pig iron is 85%; when the copper content of the superfine atomized iron powder is required to be between 0.011 percent and 0.014 percent, the content of scrap steel is 50 percent, and the content of pig iron is 50 percent; when the copper content of the superfine atomized iron powder is required to be more than 0.015 percent, the content of scrap steel is 100 percent, and the content of pig iron is 0.
According to the proportion, the use requirement can be met, when the copper content of the superfine atomized iron powder to be produced is higher, the content of pig iron is reduced, the cost is reduced, and the waste steel can be effectively utilized, so that the purposes of waste utilization and resource saving are achieved.
Step two, smelting: smelting scrap steel or pig iron or a mixture thereof in an electric arc furnace by using electric energy and chemical energy, wherein the smelting time is 130-160 minutes, the tapping temperature is 1700-1800 ℃, and mixed molten metal is formed after smelting;
the electric arc furnace has greater process flexibility than other steel-making furnaces, can effectively remove impurities such as sulfur, phosphorus and the like, is easy to control the furnace temperature, has small floor area of equipment, and is suitable for smelting high-quality alloy steel;
meanwhile, carbon powder, fluorite and lime are also required to be added in the smelting process, and 20-40 kg of the carbon powder, 150-220 kg of the fluorite and 600-900 kg of the lime are added according to the parts by weight. The carbon powder reducing agent can effectively reduce the Gr content in the metal solution by adding carbon powder into the electric arc furnace.
Lime and fluorite are important additives in the steel smelting process. The lime can prevent the excessive heat dissipation on the surface of the molten metal in the electric arc furnace, the melting is fast, and the slagging is easy, thereby improving the desulfurization and dephosphorization efficiency. The cooling effect of lime is similar to that of steel scrap, and the slag amount is large when the lime consumption is large, so that the blowing time is long, and the end point temperature is influenced. Through continuous experiments, the invention determines that when 20-40 kg of the carbon powder, 150-220 kg of fluorite and 600-900 kg of lime are added according to the parts by weight, less impurities are generated in the molten metal, the requirements of metallurgical reaction at each period in the furnace can be met, and the temperature at the end point can be accurately controlled.
Fluorite can be used as a furnace washing agent, and the effect of removing furnace wall accretions is achieved by reducing the melting point; in the smelting process, the slag fluxing agent is used as a fluxing agent, so that the melting point of lime can be reduced, the fluidity of slag is improved, and the desulfurization efficiency is improved.
Step three, water atomization: the smelted mixed liquid is impacted into particles with the diameter less than or equal to 100 microns through an atomization system, and powder slurry is formed, the water pressure of the atomization system is 15-20 MPa, and the water flow is 140-160 m 3 /h;
The invention adopts a Romanian high-pressure water atomization system, and further improves the Romanian high-pressure water atomization system, and the improved water spray system has the following advantages: the nozzle of rotation type can make the spray area increase of water smoke, has improved the production efficiency of iron powder, has reduced manufacturing cost.
The nozzle cascade seam is wide too, and the particle diameter that can make water smoke is great, and the nozzle cascade seam is wide too narrowly, can make the water smoke blowout unsmooth. The invention combines the width of the nozzle ring and the water pressure and water flow of the atomizing system, so that the particle size and penetrating power of the atomized water are excellent, and the production is well satisfied.
Water pressure is big, and it is big to make the penetrating power, and water flow is big, and the ejection rate that can make steam is high, and water pressure and water flow in the certain limit combine, can make mixed liquid obtain the abundant impact of water smoke, form more fine and close granule.
The carbon dioxide of specific velocity of flow is passed through to the nozzle front end for carbon dioxide forms supercritical state, when carbon dioxide combines with the water smoke with specific velocity of flow, can make water smoke refine and even more, further makes the iron powder dispersed into the particle size more easily littleer, more homogeneous granule. The distance that carbon dioxide lets in the water smoke is too close, can have certain influence to the velocity of flow and the pressure of water smoke, if the distance is too far away, can not play fine dispersion effect to the water smoke again. The supercritical carbon dioxide is added, so that the adopted water amount is reduced, the production efficiency is improved, the production cost is reduced, and the energy is saved. On the other hand, free carbon dioxide is used, so that carbon neutralization is realized while the production cost is saved and the energy consumption is reduced.
Harmful gases generated during the production of iron powder can be absorbed by supercritical carbon dioxide. The supercritical carbon dioxide fluid is colorless, tasteless and nontoxic in a normal state, has no solvent residue after being separated from the extracted components, can effectively avoid the solvent toxicity residue under the traditional solvent extraction condition, simultaneously prevents the toxicity of the extraction process to human bodies and the pollution to the environment, and is a natural and environment-friendly extraction technology.
The molten steel with low chemical components is impacted into fine particles with the diameter less than or equal to 100 microns, so that the production efficiency and the product quality performance are obviously improved. The diameter of the zirconium core of the atomization system is 16mm, the diameter of the zirconium core commonly used in the market is about 80mm at present, and the diameter of the zirconium core of the atomization system is far smaller than that of the zirconium core currently used in the market, so that molten steel can be effectively prevented from leaking, and the service life of equipment is prolonged. The nozzle angle is 11 deg. so that it provides a large striking force per unit area to impact the low chemical composition molten steel into fine particles.
Step four, dehydration and drying: the atomized slurry passes through a wet magnetic separator to enable the slurry containing iron powder to be adsorbed on a magnetic roller, part of nonmagnetic impurities are removed through washing of water, then the moisture in the slurry is extracted through a vacuum filter to enable the moisture content of the rest powder to be lower than 13%, then the powder is dried through a drying furnace, and then the dried powder is cooled through a water-cooling trough to enable the temperature of detected iron powder to be not more than 100 ℃;
in the invention, the vacuum pressure of the vacuum filter in the fourth step is-0.02 to-0.08 Mpa, and the rotating speed of the vacuum filter is 150 to 300r/min. The water in the powder slurry is extracted through the vacuum filter, so that the water content of the rest powder is lower than 13%, and when the water content is higher than 13%, the time for drying the powder through the drying furnace is greatly prolonged, the production time is prolonged, and the production cost is increased. Through continuous experiments, the exhaust temperature of the drying furnace in the fourth step is optimally required to be 130-150 ℃. When the exhaust temperature of the drying furnace is more than 150 ℃, the thermal efficiency of the boiler is reduced, the fuel cost is increased, and the machine can not run economically; when the exhaust temperature of the drying furnace is required to be lower than 130 ℃, the heating area of the boiler is increased, the resistance of a smoke air duct is increased, and the power consumption of a fan is increased.
Step five, sieving and magnetic separation: conveying the dried powder to a screening machine through a bucket elevator for screening, and removing nonmagnetic impurities from the screened powder through a dry magnetic separator to obtain superfine atomized iron powder;
in the invention, the screening machine in the fifth step adopts a 100-mesh screen. During screening, the materials above the screen are separately connected with bags for isolation, and the materials below the screen pass through a dry magnetic separator to remove nonmagnetic impurities, so that the superfine atomized iron powder is obtained.
Step six, packaging and delivering: and packaging the obtained superfine atomized iron powder to ensure that the bag is not damaged and the label is put well.
The specific embodiment is as follows:
example one
A production process of superfine atomized iron powder for a new energy battery comprises the following preparation methods:
step one, charging: 5t of pig iron is added into an electric arc furnace;
step two, smelting: smelting pig iron in an electric arc furnace by using electric energy and chemical energy, wherein 25kg of carbon powder, 185kg of fluorite and 800kg of lime are added according to parts by weight in the smelting process, the smelting time is 160 minutes, the tapping temperature is 1750 ℃, and molten metal is formed after smelting;
step three, water atomization: the adopted nozzle is rotary, and the rotating speed is 300r/min; the width of the nozzle ring seam is 0.3mm; the water pressure of the atomization system is 15Mpa, and the water flow is 140m 3 H; the atomization temperature is 1400 ℃; at the front end of the nozzle, carbon dioxide gas passes through the nozzle, the specific flow rate is 3L/min, the diameter of a zirconium core of an atomization system is 16mm, the angle of the nozzle is 11 degrees, and the smelted mixed liquid metal liquid is impacted into particles with the diameter less than or equal to 100 micrometers through the atomization system to form powder slurry;
step four, dehydration and drying: the atomized slurry is firstly subjected to a wet magnetic separator to enable the slurry containing iron powder to be adsorbed on a magnetic roller, part of nonmagnetic impurities are removed through washing of water, then the atomized slurry is subjected to a vacuum filter, the vacuum pressure of the vacuum filter is-0.02 to-0.08 Mpa, the rotating speed of the vacuum filter is 150 to 300r/min, the vacuum filter extracts water in the slurry, the water content of the rest powder is lower than 13 percent, then the powder is dried through a drying furnace, the exhaust temperature of the drying furnace is required to be 130 to 150 ℃, and then the dried powder is subjected to cooling treatment through a water cooling material tank, so that the temperature of detected iron powder is not higher than 100 ℃;
step five, sieving and magnetic separation: conveying the dried powder to a screening machine for screening by a bucket elevator, wherein the screening machine adopts a 100-mesh screen, and the screened powder passes through a dry magnetic separator to remove nonmagnetic impurities so as to obtain superfine atomized iron powder;
step six, packaging and delivering: and packaging the obtained superfine atomized iron powder to ensure that the bag is not damaged and the label is put well.
Example two
Similar to the first embodiment, the differences are as follows:
step one, charging: 0.75t of scrap and 4.25t of pig iron were added to an electric arc furnace;
step two, smelting: smelting pig iron in an electric arc furnace by using electric energy and chemical energy, adding 35kg of carbon powder, 180kg of fluorite and 700kg of lime in parts by weight in the smelting process, smelting for 152 minutes, tapping at 1723 ℃, and forming molten metal after smelting.
EXAMPLE III
Similar to the first embodiment, the differences are as follows:
step one, charging: adding 5t of scrap steel into an electric arc furnace;
step two, smelting: smelting pig iron in an electric arc furnace by using electric energy and chemical energy, adding 40kg of carbon powder, 160kg of fluorite and 680kg of lime in parts by weight in the smelting process, smelting for 145 minutes, tapping at the temperature of 1750 ℃, and forming molten metal after smelting.
Example four:
similar to the first embodiment, the differences are as follows:
step three, water atomization: the adopted nozzle is rotary, and the rotating speed is 400r/min; the width of the nozzle ring seam is 0.4mm; the water pressure of the atomization system is 18Mpa, and the water flow is 150m 3 H; the atomization temperature is 1600 ℃; carbon dioxide gas passes through the front end of the nozzle at a distance of 10 cm, the specific flow rate is 4L/min, the diameter of a zirconium core of an atomization system is 16mm, the nozzle angle is 11 degrees, the smelted mixed liquid metal liquid passes through the atomization system, and is impacted into particles with the diameter less than or equal to 100 micrometers, and powder slurry is formed.
EXAMPLE five
Similar to the first embodiment, the differences are as follows:
step three, water atomization: the adopted nozzle is rotary, and the rotating speed is 500r/min; the width of the nozzle ring seam is 0.5mm; the water pressure of the atomization system is 20MPa, and the water flow is 160m 3 H; the atomization temperature is 1800 ℃; at the 10 cm position of the front end of the nozzle, carbon dioxide gas passes through the nozzle, the specific flow rate is 5L/min, the diameter of a zirconium core of an atomization system is 16mm, and the angle of the nozzle is 11 degrees. And (3) impacting the smelted mixed liquid metal liquid into particles with the diameter less than or equal to 100 micrometers through an atomization system, and forming powder slurry.
Comparative example 1
A production process of iron powder for a new energy battery comprises the following preparation method:
step one, charging: 5t of pig iron is added into an electric arc furnace;
step two, smelting: smelting pig iron in an electric arc furnace by using electric energy and chemical energy, wherein 25kg of carbon powder, 185kg of fluorite and 800kg of lime are added according to parts by weight in the smelting process, the smelting time is 160 minutes, the tapping temperature is 1750 ℃, and molten metal is formed after smelting;
step three, dehydration and drying: the atomized slurry is firstly subjected to a wet magnetic separator to enable the slurry containing iron powder to be adsorbed on a magnetic roller, part of nonmagnetic impurities are removed through washing of water, then the atomized slurry is subjected to a vacuum filter, the vacuum pressure of the vacuum filter is-0.02 to-0.08 Mpa, the rotating speed of the vacuum filter is 150 to 300r/min, the vacuum filter extracts water in the slurry, the water content of the rest powder is lower than 13 percent, then the powder is dried through a drying furnace, the exhaust temperature of the drying furnace is required to be 130 to 150 ℃, and then the dried powder is subjected to cooling treatment through a water cooling material tank, so that the temperature of detected iron powder is not higher than 100 ℃;
step four, sieving and magnetic separation: conveying the dried powder to a screening machine for screening by a bucket elevator, wherein the screening machine adopts a 100-mesh screen, and the screened powder passes through a dry magnetic separator to remove nonmagnetic impurities so as to obtain superfine atomized iron powder;
step five, packaging and delivering goods: and packaging the obtained superfine atomized iron powder to ensure that the bag is not damaged and the label is put well.
Comparative example No. two
Similar to the comparative example one, the differences are as follows:
step one, charging: 0.75t of scrap and 4.25t of pig iron were added to an electric arc furnace;
step two, smelting: smelting pig iron in an electric arc furnace by using electric energy and chemical energy, adding 35kg of carbon powder, 180kg of fluorite and 700kg of lime according to parts by weight in the smelting process, smelting for 152 minutes, tapping at 1723 ℃, and forming molten metal after smelting;
comparative example No. three
Similar to the first comparative example, the differences are as follows:
step one, charging: adding 15t of scrap steel into an electric arc furnace;
step two, smelting: smelting pig iron in an electric arc furnace by using electric energy and chemical energy, adding 40kg of carbon powder, 160kg of fluorite and 680kg of white ash in parts by weight in the smelting process, smelting for 145 minutes, tapping at the temperature of 1750 ℃, and forming molten metal after smelting;
comparative example No. four
Similar to the comparative example one, the differences are as follows:
step one, charging: 5t of commercially pure iron was added to the electric arc furnace;
comparative example five
Similar to the first comparative example, the differences are as follows:
the atomized slurry is directly filtered by a vacuum filter and is not screened by a wet magnetic separator.
Comparative example six
The differences from the first embodiment are as follows:
step three, water atomization: the adopted nozzle is rotary, and the rotating speed is 600r/min; the width of the nozzle ring seam is 0.7mm; the water pressure of the atomization system is 12MPa, and the water flow is 150m 3 H; the atomization temperature is 1200 ℃; carbon dioxide gas is fed at the front end of the nozzle with the specific flow rate of 2L/min, the diameter of a zirconium core of an atomization system is 11mm, and the angle of the nozzle is 15 degrees; and (3) impacting the smelted mixed liquid metal liquid into particles through an atomization system, and forming powder slurry.
Comparative example seven
The differences from the first embodiment are as follows:
step three, water atomization: the adopted nozzle is rotary, and the rotating speed is 300r/min; the width of the nozzle ring seam is 0.3mm; the water pressure of the atomization system is 15MPa, and the water flow is 140m 3 H; the atomization temperature is 1400 ℃; the zirconium core of the atomization system has a diameter of 16mm and a nozzle angle of 11 deg.. And (3) impacting the smelted mixed liquid metal liquid into particles with the diameter less than or equal to 100 micrometers through an atomization system, and forming powder slurry.
Test section
(1) Detection of metal chemical composition
Testing an instrument: spectrometer
Test reference standard: ASTM E1086, instructions for work: HCBZ-SW-LAB-005
Test samples: iron powder in example one, example two, example three, comparative example one, comparative example two, comparative example three, comparative example four, and comparative example five.
The test method comprises the following steps: and (3) sequentially weighing 0.60g of the test sample, 6.00g of lithium tetraborate solvent, 0.03g of ammonium iodide and 1.00g of cobalt carbonate powder, uniformly mixing, melting for 20min, taking out, pouring the sample into a mold, horizontally standing and cooling, taking down the melt piece, and placing the melt piece into a dryer for marking for later use.
And (3) carrying out X fluorescence intensity detection on the sample successively, drawing a content and intensity curve, and measuring the sample.
(2) Particle size distribution detection
Testing an instrument: screening machine and balance
Test reference standard: MPIF Standard 05, job instruction: HCBZ-SW-LAB-029
Test samples: iron powder in example one, example two, example three, example four, example five, comparative example one, comparative example two, comparative example three, comparative example four, comparative example five, comparative example six, and comparative example seven.
The test method comprises the following steps: and weighing 100g of the test samples by using a balance, placing the test samples on a screening machine for screening in sequence, wherein the screening machine adopts a 100-mesh screen, and recording results after screening.
The test results are shown in Table 1
Figure BDA0003999051480000151
Figure BDA0003999051480000161
As can be seen from table 1, when the metal elements in the first example are compared with those in the first comparative example, the fourth comparative example and the fifth comparative example, the metal elements in the second example are compared with those in the second comparative example, and the metal elements in the third example are compared with those in the third comparative example, the iron content in the first example is the highest and reaches 99.8%, meanwhile, the chromium content is 0.012% and is less than 0.015%, the manganese content is 0.040% and is less than 0.08%, the market demand is met, the copper content is 0.0023% and is less than 0.003%, the market demand is met, the product produced by the first example meets the market demand and fills the blank of the existing market; the contents of iron, chromium, manganese and copper in the first comparative example, the fourth comparative example and the fifth comparative example can not meet the market demand; secondly, the content of iron in the second example reaches 99.4 percent, and the copper content does not exceed 0.010 percent, while the content of iron in the second comparative example is 97.4 percent, the iron content is lower, and the copper content is higher and exceeds 0.010 percent, so that the requirement is not met; the iron content in example three was 99.0% and the copper content was 0.015%, whereas the iron content in comparative example three was 97.8%, the copper content was 0.086%, the iron content in comparative example three was significantly lower than the iron content in example three, whereas the copper content in comparative example three was significantly higher than the copper content in example three; therefore, the application provides a superfine atomizing iron powder production technology for new energy battery through dehydration drying and sieving magnetic separation two steps, gets rid of non-magnetic impurity, has improved the purity of product, has reduced the content of chromium, manganese, copper.
Compared with the particle size distribution in the first, second, third, fourth and fifth comparative examples, the particle size distribution of the products in the first, second and third examples is uniform, the particle size distribution of the products in the first, second and third examples can reach 99.7% under a 100-mesh sieve, while the particle size distribution of the products in the first, second, third and fourth comparative examples is not too uniform, the particle size distribution of the products in the second, third and fourth comparative examples can reach more than 60% under the 100-mesh sieve, and the fifth comparative example has more nonmagnetic impurities and non-uniform particle size distribution and can not reach 50% under the 100-mesh sieve due to the fact that the products are not screened by a wet magnetic separator, so that the fine powder produced by the superfine atomized iron powder production process is higher in content, obvious in product yield effect and lower in manufacturing cost, and the product particle composition and chemical performance of the iron phosphate are more stable, and the superfine atomized iron phosphate produced by the new energy battery produced by the production process is free of by producing by byproducts, short in process time and high in product purity, and the process of changing the chemical preparation that the nitric acid or sulfuric acid is dissolved by using the complex process, and has no pollution to the environment; the production process is simple and convenient, easy to operate and high in practicability. The novel steel-making two-line device is improved and optimized, so that the pollution of impurities is avoided, the cleanliness of the product is ensured, the metal powder can be effectively subjected to centralized treatment and collection, the resources are effectively saved, the working efficiency is improved, and the service life of the device is prolonged.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Claims (10)

1. A production process of superfine atomized iron powder for new energy batteries is characterized by comprising the following steps: the preparation method comprises the following steps:
step one, charging: one or two of scrap steel or pig iron are added into an electric arc furnace according to a proportion;
step two, smelting: smelting scrap steel or pig iron or a mixture thereof in an electric arc furnace by using electric energy and chemical energy, wherein the smelting time is 130-160 minutes, the tapping temperature is 1700-1800 ℃, and mixed molten metal is formed after smelting;
step three, water atomization: in the atomization system, the adopted nozzle is rotary, and the rotating speed is 300-500 r/min; the width of the nozzle ring seam is 0.3-0.5 mm; the water pressure of the atomization system is 15-20 MPa, and the water flow is 140-160 m 3 H; the atomization temperature is 1400-1800 ℃; at the 10 cm position of the front end of the nozzle, carbon dioxide gas is passed through the nozzle, the specific flow rate is 3-5L/min, and the smelted mixed liquid is impacted into particles with the diameter less than or equal to 100 micrometers by an atomization system, so that powder slurry is formed.
Step four, dehydration and drying: the atomized slurry passes through a wet magnetic separator to enable the slurry containing iron powder to be adsorbed on a magnetic roller, part of nonmagnetic impurities are removed through washing of water, then the moisture in the slurry is extracted through a vacuum filter to enable the moisture content of the rest powder to be lower than 13%, then the powder is dried through a drying furnace, and then the dried powder is cooled through a water-cooling trough to enable the temperature of detected iron powder to be not more than 100 ℃;
step five, sieving and magnetic separation: conveying the dried powder to a screening machine through a bucket elevator for screening, and removing nonmagnetic impurities from the screened powder through a dry magnetic separator to obtain superfine atomized iron powder;
step six, packaging and delivering goods: and packaging the obtained superfine atomized iron powder to ensure that the bag is not damaged and the label is put well.
2. The production process of the superfine atomized iron powder for the new energy battery as claimed in claim 1, wherein the production process comprises the following steps: the purity of the pig iron in the first step is 99.990-99.997%.
3. The production process of the superfine atomized iron powder for the new energy battery as claimed in claim 1, wherein the production process comprises the following steps: the proportion of the scrap steel or/and the pig iron in the first step is as follows: when the copper content of the superfine atomized iron powder is less than 0.006 percent, the content of the scrap steel is 0, and the content of the pig iron is 100 percent; when the copper content of the superfine atomized iron powder is required to be between 0.007 and 0.010 percent, the content of the scrap steel is 15 percent, and the content of the pig iron is 85 percent; when the copper content of the superfine atomized iron powder is required to be between 0.011 percent and 0.014 percent, the content of scrap steel is 50 percent, and the content of pig iron is 50 percent; when the copper content of the superfine atomized iron powder is required to be more than 0.015 percent, the content of scrap steel is 100 percent, and the content of pig iron is 0.
4. The production process of the superfine atomized iron powder for the new energy battery as claimed in claim 1, wherein the production process comprises the following steps: the electric arc furnace adopted in the step one or the step two is a 15-ton electric arc furnace.
5. The production process of the superfine atomized iron powder for the new energy battery as claimed in claim 1, wherein the production process comprises the following steps: carbon powder, fluorite and lime are also required to be added in the smelting process in the second step.
6. The production process of the superfine atomized iron powder for the new energy battery as claimed in claim 1, wherein the production process comprises the following steps: 20-40 kg of carbon powder, 150-220 kg of fluorite and 600-900 kg of lime are added according to the weight parts.
7. The production process of the superfine atomized iron powder for the new energy battery according to claim 1, wherein the production process comprises the following steps: in the third step, the diameter of the zirconium core of the atomization system is 16mm, and the angle of the nozzle is 11 degrees.
8. The production process of the superfine atomized iron powder for the new energy battery as claimed in claim 1, wherein the production process comprises the following steps: the vacuum pressure of the vacuum filter in the fourth step is-0.02 to-0.08 Mpa, and the rotating speed of the vacuum filter is 150 to 300r/min.
9. The production process of the superfine atomized iron powder for the new energy battery according to claim 1, wherein the production process comprises the following steps: the exhaust temperature of the drying furnace in the fourth step is required to be 130-150 ℃.
10. The production process of the superfine atomized iron powder for the new energy battery as claimed in claim 1, wherein the production process comprises the following steps: and the screening machine in the fifth step adopts a 100-mesh screen.
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