CN110170646B - Superfine iron powder and its production process - Google Patents
Superfine iron powder and its production process Download PDFInfo
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- CN110170646B CN110170646B CN201910584533.1A CN201910584533A CN110170646B CN 110170646 B CN110170646 B CN 110170646B CN 201910584533 A CN201910584533 A CN 201910584533A CN 110170646 B CN110170646 B CN 110170646B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to the technical field of metal waste pretreatment, and particularly relates to superfine iron powder. The granularity D50 of the iron powder is less than or equal to 20 mu m, the iron content is more than or equal to 97 percent, and the loose specific gravity is 0.5-1.5g/cm 3. The iron powder of the invention has small granularity, high purity and small loose specific gravity.
Description
Technical Field
The invention belongs to the technical field of metal waste pretreatment, and particularly relates to superfine iron powder and a production method thereof.
Background
Iron powder is one of basic raw materials in the powder metallurgy industry, and the annual worldwide yield of iron powder is about 85 million tons. 85% of the iron powder production is used for the manufacture of powder metallurgy parts, with 70% -83% of the powder metallurgy parts being used in the automotive industry. The rest of the iron powder is used for chemical industry, magnetic materials, cutting, welding rods, heating materials and the like (from the iron powder production condition, the development trend of domestic iron powder, Kudzuvine, the powder industry of China, No. 2 in 2006, page 40, abstract lines 1-3, and published 2006, 12 months and 31 days).
For iron powder, the finer the iron powder, the larger the specific surface area and the stronger the activity, so that the iron powder has stronger electric, magnetic, optical and special performances such as catalysis, adsorption and chemical reaction, and therefore has a wide application prospect in various fields such as electromagnetism, biology, medicine and optics (research progress on low-temperature reduction for preparing ultrafine iron powder, korean yilin and the like, shanghai metal, vol.32, No. 1, p.47, lines 4-7, published year 2010, year 01, month 31). Therefore, the ultrafine iron powder is widely applied to the fields of magnetic materials, medicines, foods, manufacturing of welding rods, automobile exhaust treatment, chemical industry, metallurgy, superhard materials, hard alloys, high-density alloys, mechanical equipment, coatings, pigments for rubber products, seed optimization, seed purification, soil improvement and the like ("the current situation and progress of application research of ultrafine iron powder", wushahua et al, yunnan metallurgy and the like, 34 th 5 of volume 2005, 1 st line of the last 1 st section of the left column of page 34, 2 nd lines of the right column of page 34, 2 rd lines of the 3 rd sections of the right column of page 34, and 2 nd lines of the 2 nd sections of the left column of page 35, 1 st line of the 35 th section of page 35, and 10 months and 31 days of publication 2010).
However, the existing iron powder has a coarse particle size (D50 is more than 45um), which reduces the surface activity thereof, increases the sintering temperature and affects the structural performance of the product; the pressing pressure of the pressed blank is increased, and the burden of a die is increased; meanwhile, the surface roughness of the product is increased, and the processing precision of parts is reduced; in addition, the magnetic properties, catalytic properties, and other special properties of the catalyst in other fields are reduced, and the application fields are limited.
Disclosure of Invention
In view of the above, an object of the present invention is to provide an iron powder having a small particle size.
In order to achieve the purpose, the technical scheme of the invention is as follows:
iron powder, wherein the particle size D50 of the iron powder is less than or equal to 20 mu m, the iron content is more than or equal to 97 percent, and the loose specific gravity is 0.5-1.5g/cm3。
The D50 refers to the corresponding particle size when the cumulative percentage of particle size distribution reaches 50%, i.e., 50% of the particles larger than the particle size and 50% of the particles smaller than the particle size.
The loose specific gravity refers to the mass per unit volume measured after iron powder is freely filled in a standard container.
Furthermore, the particle size D90 of the iron powder is less than or equal to 40 μm.
The particle size D90 refers to the corresponding particle size when the cumulative percentage of particle size distribution reaches 90%, i.e. the particles smaller than the particle size account for 90%.
In addition, the inventor also finds that the iron-based composite powder is produced by utilizing the principle that Fe + Cu performs a chemical replacement reaction on iron powder and copper sulfate solution under the condition of certain additives2+→Fe2++ Cu produces great amount of waste liquid containing high concentration ferrous ion, and the waste liquid reacts with liquid alkali to produce iron containing waste slag and Fe2++2OH-=Fe(OH)2↓. At present, a large amount of iron-containing waste residues are subjected to pressure filtration by a pressure filter, filter residues are removed by a factory, and a certain cost is paid to the factory. This treatment wastes iron resources and increases the cost of wastewater treatment.
The second purpose of the invention is to protect the preparation method of the iron powder, which comprises the following steps:
washing, roasting, crushing, reducing, crushing and winnowing the iron-containing waste residues generated in the production of the iron-based composite powder in sequence, wherein the reducing temperature is 800-1000 ℃, the time is 130-170min, and the introduction amount of hydrogen is 1.5-3.0m3/h。
Further, the washing refers to processing the iron-containing waste residue, putting the iron-containing waste residue into a filtering-washing integrated machine, adding water for washing for 5 hours, and then performing pressure filtration until the water content is less than or equal to 20%.
Further, the roasting temperature is 700-3/h。
Furthermore, the crushing refers to crushing until the particle size D97 is less than or equal to 5 μm.
Further, the preparation method of the iron powder comprises the following specific steps: washing, roasting, crushing, reducing, crushing and winnowing the iron-containing waste residues generated in the production of the iron-based composite powder in sequence, wherein the washing refers to processing the iron-containing waste residues, putting the processed iron-containing waste residues into a filtering-washing integrated machine, adding water for washing for 5 hours, and then performing filter pressing until the water content is less than or equal to 20%; the roasting temperature is 700-800 ℃, the roasting time is 80-100min, and the air inlet amount is 2-4m3H; the crushing refers to crushing until the particle size D97 is less than or equal to 5 mu m; the reduction temperature is 800-1000 ℃, the time is 130-170min, and the hydrogen introduction amount is 1.5-3.0m3/h。
The invention has the beneficial effects that:
the iron powder has small particle size, the particle size D50 is less than or equal to 20 mu m, and the particle size D97 is less than or equal to 40 mu m.
The iron powder has high purity up to 97%.
The iron powder of the invention has small apparent density.
The invention realizes the recycling of iron resources and reduces the cost.
Detailed Description
The examples are provided for better illustration of the present invention, but the present invention is not limited to the examples. Therefore, those skilled in the art should make insubstantial modifications and adaptations to the embodiments of the present invention in light of the above teachings and remain within the scope of the invention.
The following detection method for water content is as follows: taking a certain amount of iron powder, putting the iron powder into a vacuum drying oven, drying the iron powder for 2 hours at the temperature of 105-110 ℃, reducing the temperature to room temperature, relieving pressure, taking out the iron powder and weighing the iron powder, and calculating the weight difference between the iron powder and the weight difference;
detecting the following particle sizes by using a laser particle size analyzer;
detecting the following iron content according to GB/T223.7-2002 potassium dichromate titration method for determining iron content of iron powder;
the loose specific gravity was measured in accordance with GB/T1479.1-2011 part 1 funnel method for measuring the loose density of metal powder.
Example 1
The preparation method of the superfine iron powder comprises the following steps:
A. washing: putting the iron-containing waste residue (with water content of 40%) into a filtering-washing integrated machine, adding water for washing for 5 hours, and then carrying out pressure filtration until the water content is less than or equal to 20% to obtain a pressure filtration block;
B. roasting: loading the washed filter pressing blocks into a burning boat, feeding into a mesh belt furnace at 800 deg.C, and introducing 3m air3Roasting for 90min under the condition of/h to obtain a block;
C. crushing: crushing the block obtained by roasting in a grading impact mill to obtain a particle size D97(D97 refers to the corresponding particle size when the cumulative particle size distribution percentage reaches 97%, namely, the particle size is smaller than 97%) to obtain powder;
D. reduction: c, putting the powder obtained in the step C into a burning boat, and sending the powder into a mesh belt furnace at the temperature of 900 ℃ with the introduction amount of hydrogen being 1.5m3Reduction treatment for 150min under the condition of/h;
E. crushing and winnowing: and placing the iron powder obtained by reduction treatment in a fluidized bed scattering classifier for crushing and air separation.
Performance testing
The iron obtained by the crushing treatment in example 1 was subjected to the property tests in terms of the particle sizes D50 and D90, the iron content, the apparent specific gravity, and the like, and the results are shown in table 1.
TABLE 1 Performance test results
As is clear from Table 1, the iron powder obtained in example 1 had a particle size D50 of 19 μm, a D90 of 37 μm, and a bulk specific gravity of 1.238g/cm3. Thus, the iron powder of the invention has small granularity and small apparent density,the purity is high.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (2)
1. The preparation method of the iron powder is characterized in that the iron-containing waste residue generated in the production of the iron-based composite powder is washed, roasted, crushed, reduced, crushed and winnowed in sequence, wherein the washing refers to processing the iron-containing waste residue and placing the processed iron-containing waste residue into a filtering-washing integrated machine, adding water for washing for 5 hours, and then performing filter pressing until the water content is less than or equal to 20 percent; the roasting temperature is 800 deg.C, the roasting time is 90min, and the air inlet amount is 3m3H; the crushing refers to crushing until the particle size D97 is less than or equal to 5 mu m; the reduction temperature is 900 ℃, the time is 150min, and the introduction amount of hydrogen is 1.5m3H; the particle size D50 of the iron powder is less than or equal to 20 mu m, the iron content is more than or equal to 97 percent, and the loose specific gravity is 0.5-1.5g/cm3。
2. The method of claim 1, wherein the iron powder has a particle size D90 ≤ 40 μm.
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CN102091788B (en) * | 2010-11-23 | 2013-07-17 | 北京科技大学 | Method for industrially producing iron-based dispersion-strengthened material |
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CN105817640A (en) * | 2016-03-28 | 2016-08-03 | 无锡市飞云球业有限公司 | Production process for manufacturing reduced iron powder with steel ball grinding iron cement |
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CN108080649A (en) * | 2017-12-14 | 2018-05-29 | 新冶高科技集团有限公司 | A kind of method that hydrocarbon duplex reduction of low temperature prepares superfine iron powder |
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