WO2020096293A1 - Procédé de fabrication de poudre d'éponge de fer en forme d'aiguille ou en forme de tige et poudre d'éponge de fer en forme d'aiguille ou en forme de tige ainsi fabriquée - Google Patents

Procédé de fabrication de poudre d'éponge de fer en forme d'aiguille ou en forme de tige et poudre d'éponge de fer en forme d'aiguille ou en forme de tige ainsi fabriquée Download PDF

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Publication number
WO2020096293A1
WO2020096293A1 PCT/KR2019/014795 KR2019014795W WO2020096293A1 WO 2020096293 A1 WO2020096293 A1 WO 2020096293A1 KR 2019014795 W KR2019014795 W KR 2019014795W WO 2020096293 A1 WO2020096293 A1 WO 2020096293A1
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WIPO (PCT)
Prior art keywords
ferric
iron powder
powder
needle
shaped
Prior art date
Application number
PCT/KR2019/014795
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English (en)
Korean (ko)
Inventor
한길수
엄형섭
박진균
Original Assignee
주식회사 포스코
재단법인 포항산업과학연구원
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by 주식회사 포스코, 재단법인 포항산업과학연구원 filed Critical 주식회사 포스코
Priority to EP19881941.9A priority Critical patent/EP3878580A4/fr
Priority to JP2021523261A priority patent/JP2022506098A/ja
Priority to CN201980072505.XA priority patent/CN112969544A/zh
Priority to US17/290,677 priority patent/US20220008992A1/en
Publication of WO2020096293A1 publication Critical patent/WO2020096293A1/fr

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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
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/062—Fibrous particles
    • 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
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/01—Reducing atmosphere
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/01—Reducing atmosphere
    • B22F2201/013—Hydrogen
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/03—Oxygen
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/04—CO or CO2
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention provides a method for manufacturing a needle or rod-shaped porous iron powder, and a needle or rod-shaped porous iron powder produced thereby. More specifically, the present invention provides a method for producing a needle-shaped or rod-shaped porous iron powder using an aqueous solution of ferric chloride, and a needle-shaped or rod-shaped porous iron powder produced thereby.
  • the conventional method for manufacturing iron powder is 1) a sponge-iron process (sponge-iron process) and a water-atomizing process.
  • the sponge-iron process is a process of reducing iron oxide to form a porous iron powder
  • the water spray process is an atomizing process of molten iron using a high-pressure water jet, wherein the iron powder produced at this time is It is a dense powder that is not porous. Also, most of the powders produced in this way have an angular cube shape, a spherical shape, or a heterogeneous shape.
  • the iron oxide used in the sponge-iron process can be used as a raw material such as iron ore or powder generated during the ironmaking process, iron oxide produced using a pickling solution generated after surface pickling during the iron plate manufacturing process, and produced by the sponge-iron process
  • Porous iron powder is characterized by a large specific surface area, high reactivity, and strong reducibility, making it a self-lubricating bearings material; Soil, groundwater, industrial wastewater purification materials (catalysts, reducing agents, etc.); Welding rod coating material; Pocket stove material; Deoxidizers; Raw materials for the production of iron compounds; It can be used in places such as extractants for cementation.
  • US Patent Publication No. 2016-0096739 uses a process for producing iron powder through an aqueous solution of ferric chloride, but when a method of manufacturing a needle or rod-shaped porous iron powder from an aqueous solution of ferric chloride is developed, iron powder is used. It is expected to be more useful in the field of use.
  • One aspect of the present invention is to provide a method for manufacturing an iron powder having both needle-like or rod-like features and porous characteristics.
  • it is to provide an iron powder produced by the manufacturing method of the present invention.
  • a ferrous chloride aqueous solution is concentrated to prepare ferrous dihydride; Preparing the ferric dihydrate powder by solid-liquid separation of the ferric dichloride; Oxidizing the ferric dihydrate powder; And it provides a needle or rod-shaped porous iron powder manufacturing method comprising the step of reducing the oxidized ferric monohydrate.
  • a needle or rod-shaped porous iron powder produced by the above manufacturing method is provided.
  • the process of the present invention it is possible to mass-produce iron powder from an aqueous solution of iron chloride, and the iron powder thus manufactured has a porous needle-like or rod-like shape, and thus can be used in the existing application of porous iron powder, as well as of rod-like powder It is possible to obtain an improvement in filling rate based on characteristics, improvement in workability, and improvement in physical properties.
  • FIG. 1 shows a schematic flow chart of a method for manufacturing a needle or rod-shaped porous iron powder of the present invention.
  • Figure 2 shows an image taken by SEM of ferric dichloride and ferrous tetrachloride crystals that appear when the ferric chloride aqueous solution is concentrated according to an embodiment of the present invention.
  • Figure 3 shows an image taken by SEM of the iron oxide powder obtained after performing the roasting process on ferrous dichloride obtained by concentration of aqueous ferric chloride solution according to an embodiment of the present invention.
  • Figure 4 shows an image taken by SEM of the reduced iron powder obtained after performing a reduction reaction to the iron oxide powder according to an embodiment of the present invention.
  • the present invention provides a manufacturing method for producing iron powder having both needle-like or rod-like characteristics and porous characteristics, and an iron powder produced by the manufacturing method.
  • the method of manufacturing a needle or rod-shaped porous iron powder of the present invention comprises the steps of: concentrating an aqueous ferric chloride solution to produce ferric dihydride; Preparing the ferric dihydrate powder by solid-liquid separation of the ferric dichloride; Oxidizing the ferric dihydrate powder; And it provides a needle or rod-shaped porous iron powder manufacturing method comprising the step of reducing the oxidized ferric monohydrate.
  • the raw material of the ferric chloride aqueous solution may be a thick solution generated after the pickling process for removing oxides on the surface during the iron plate manufacturing process, a thick solution generated during other processes or an aqueous solution in which iron is dissolved in hydrochloric acid, and the ferric chloride aqueous solution is saturated or supersaturated. It is preferably an aqueous solution that is not.
  • the concentration of the aqueous ferric chloride solution is 20 to 625 g / L, preferably 250 to 600 g / L.
  • concentration is less than 20 g / L, the amount of ferric chloride in the aqueous solution is small, and thus the energy to evaporate moisture during concentration is excessively consumed, and there is also a problem that the amount of ferrous dihydride precipitated is small, and when it exceeds 625 g / L, chloride There is a problem that precipitation occurs during transport due to saturated or supersaturated aqueous solution of ferrous iron.
  • the ferric chloride aqueous solution is concentrated to precipitate supersaturated ferric dichloride, where concentration may be performed, for example, by evaporative concentration.
  • the solid-liquid separation performed in the step of preparing the ferric dihydride powder can be separated, for example, the precipitated ferric dichloride using a centrifugal separator, but is not limited thereto, filtration, and solid-liquid separation in the art It can be carried out by any method that can be used for.
  • the temperature of the concentration process should be controlled, and evaporation concentration is preferably performed at, for example, 72 to 125 ° C, preferably 75 to 95 It is carried out at a temperature of °C.
  • evaporation concentration is preferably performed at, for example, 72 to 125 ° C, preferably 75 to 95 It is carried out at a temperature of °C.
  • ferrous tetrachloride may precipitate, and the ferric tetrachloride has a problem of precipitating in the form of a rectangular polyhedron, and at temperatures exceeding 125 ° C, not only iron monochloride is generated, but energy is excessive. There is a problem to be wasted.
  • the image taken by SEM of ferric tetrachloride precipitated in the form of the polygonal polyhedron is shown in FIG. 2.
  • the step of oxidizing the ferric dihydride powder may be performed by a roasting process in which a thermal decomposition reaction is performed in an oxygen atmosphere.
  • the reaction of ferrous dihydride and oxygen in the roasting process is as follows.
  • the roasting process is not limited, but a reactor such as a flow path, a rotary kiln, a belt, or a drop tube can be used, and external force acts on the powder during the reaction. Therefore, it is necessary to minimize the crushing of the powder to maintain the shape of the rod.
  • a reactor such as a flow path, a rotary kiln, a belt, or a drop tube can be used, and external force acts on the powder during the reaction. Therefore, it is necessary to minimize the crushing of the powder to maintain the shape of the rod.
  • the reaction of the roasting process is 200 It may be carried out at a temperature of 1300 °C. This is because iron oxide is not generated below 200 ° C and iron oxide sintering occurs above 1300 ° C, making it difficult to obtain iron oxide in a desired shape. Preferably it can be carried out at a temperature of 500 to 800 °C.
  • Classification may be performed to distinguish the shape of the iron oxide generated through the roasting process. Furthermore, in the case of hydrochloric acid generated during the above process, it can be used to make a hydrochloric acid aqueous solution by wet capture to make an aqueous ferric chloride solution.
  • the step of reducing the oxidized ferric dihydrate may be performed through a reduction reaction in the high temperature reducing atmosphere.
  • the reducing atmosphere may be, for example, hydrogen, carbon monoxide or a mixed gas atmosphere thereof, and a compound capable of forming hydrogen, carbon monoxide or a mixed gas thereof through a reaction such as decomposition may be used as a reducing agent.
  • the reduction reaction is, for example, as follows.
  • the reduction reaction is not limited, but a reactor such as a flow path, a rotary kiln, a belt, or a drop tube can be used, and external force acts on the powder during the reaction. Therefore, it is necessary to minimize the crushing of the powder to maintain the shape of the rod.
  • the reduction reaction is 400 It may be carried out at a temperature of 1300 °C. Below 400 °C, the reaction rate is slow and productivity decreases. Above 1300 °C, sintering of the reduced iron generated excessively or the reduced iron microstructure is coarsened. This is because a problem arises that the porous tissue disappears.
  • the reducing atmosphere is a hydrogen atmosphere
  • the reduction reaction may be preferably performed at a temperature of 600 to 800 ° C
  • the reducing atmosphere is a carbon monoxide atmosphere
  • the reduction reaction may be preferably performed at a temperature of 700 to 1000 ° C.
  • Classification may be performed to distinguish the shape of the reduced iron generated through the reduction reaction. Furthermore, since the reduced iron produced has good reactivity and re-oxidation may occur, the powder must be collected in an inert atmosphere.
  • the specific surface area of the acicular or rod-shaped porous iron powder produced by the production method of the present invention is 0.3 to 3 m 2 / g, and preferably 0.5 to 2.5 m 2 / g.
  • the specific surface area of the iron powder is less than 0.3 m 2 / g, there is a problem of low reactivity, and when it exceeds 3 m 2 / g, oxidation or ignition occurs easily in the atmospheric state, which makes it difficult to handle during the process.
  • Needle-shaped or rod-shaped iron powders were prepared by using an aqueous solution of ferric chloride (FeCl 2 ) generated in the nickel wet smelting process.
  • An exemplary process is shown in FIG. 1, and a specific process is as follows.
  • the aqueous solution of ferric chloride (concentration is 220 g / L) was concentrated to precipitate supersaturated ferric dihydrate (FeCl 2 ⁇ 2H 2 O).
  • the precipitated ferric dichloride was subjected to solid-liquid separation by centrifugation to separate ferric dichloride powder. At this time, concentration of the aqueous solution was carried out at 80 °C temperature.
  • the ferric dihydride powder was introduced into a rotary kiln and roasted through a pyrolysis reaction in a high temperature atmosphere containing oxygen. As a result, needle or rod-shaped iron oxide is produced.
  • the roasting process was performed at 700 ° C. for 90 minutes, and classification was performed to distinguish the shape of the produced iron oxide in the form of needles or rods.
  • Fe 3 O 4 or FeO oxide may be rarely generated as well as Fe 2 O 3 .
  • HCl produced together in the rotary kiln was collected by a scrubber and reused in a nickel smelting process.
  • iron iron powder was prepared through a reduction reaction in a high-temperature gas reduction atmosphere by injecting the needle or rod-like iron oxide into a mesh belt.
  • the gas reduction atmosphere is a hydrogen or carbon monoxide atmosphere.
  • the reduction reaction was performed at 750 ° C. for 60 minutes, and classification was performed to classify the shape of the produced iron oxide in the form of needles or rods, and divided into needle or rod-shaped reduced iron powders and fine reduced iron powders.
  • the resulting needle or rod-shaped reduced iron powder was a powder having a length of about 500 ⁇ m and an expected ratio of about 5, and a specific surface area of about 2.3 m 2 / g.
  • the reactivity is good and re-oxidation may occur, so the powder must be collected in an inert atmosphere.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Compounds Of Iron (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'une poudre d'éponge de fer en forme d'aiguille ou en forme de tige. Plus précisément, la présente invention concerne un procédé de fabrication d'une poudre d'éponge de fer en forme d'aiguille ou en forme de tige et une poudre d'éponge de fer en forme d'aiguille ou en forme de tige ainsi fabriquée, le procédé comprenant les étapes suivantes consistant : à préparer un chlorure de dichlorure ferreux par concentration d'une solution aqueuse de chlorure ferreux; à séparer un solide-liquide du dichlorure ferreux pour préparer de la poudre de dichlorure ferreux; à oxyder la poudre de dichlorure ferreux; et à réduire le dichlorure ferreux oxydé.
PCT/KR2019/014795 2018-11-05 2019-11-04 Procédé de fabrication de poudre d'éponge de fer en forme d'aiguille ou en forme de tige et poudre d'éponge de fer en forme d'aiguille ou en forme de tige ainsi fabriquée WO2020096293A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP19881941.9A EP3878580A4 (fr) 2018-11-05 2019-11-04 Procédé de fabrication de poudre d'éponge de fer en forme d'aiguille ou en forme de tige et poudre d'éponge de fer en forme d'aiguille ou en forme de tige ainsi fabriquée
JP2021523261A JP2022506098A (ja) 2018-11-05 2019-11-04 針状または棒状多孔質鉄粉末の製造方法及びこれにより製造された針状または棒状の多孔質鉄粉末
CN201980072505.XA CN112969544A (zh) 2018-11-05 2019-11-04 针状或棒状多孔铁粉的制备方法及由此制备的针状或棒状多孔铁粉
US17/290,677 US20220008992A1 (en) 2018-11-05 2019-11-04 Method for manufacturing needle-shaped or rod-shaped porous iron powder and needle-shaped or rod-shaped porous iron powder manufactured thereby

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2018-0134325 2018-11-05
KR1020180134325A KR102175428B1 (ko) 2018-11-05 2018-11-05 침상 또는 봉상 다공질 철분말 제조 방법

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WO2020096293A1 true WO2020096293A1 (fr) 2020-05-14

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US (1) US20220008992A1 (fr)
EP (1) EP3878580A4 (fr)
JP (1) JP2022506098A (fr)
KR (1) KR102175428B1 (fr)
CN (1) CN112969544A (fr)
WO (1) WO2020096293A1 (fr)

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KR102477414B1 (ko) * 2022-06-08 2022-12-15 김준현 복합성능 모르타르 조성물 및 상기 복합성능 모르타르 조성물과 무기계 표면보호 코팅제를 이용한 콘크리트 및 강재 구조물의 보수보강 공법

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US20160096739A1 (en) 2014-09-29 2016-04-07 Innova Powders, Inc. Iron powder product with high specific surface area
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JP2005145757A (ja) * 2003-11-14 2005-06-09 Nisshin Steel Co Ltd 酸化鉄粉の製造方法
US20160096739A1 (en) 2014-09-29 2016-04-07 Innova Powders, Inc. Iron powder product with high specific surface area
KR101798731B1 (ko) * 2015-12-24 2017-11-17 주식회사 포스코 산화철 제조방법
KR20180082760A (ko) * 2017-01-11 2018-07-19 국방과학연구소 1차 및 2차 환원공정을 적용한 철 분말 제조방법 및 이에 의해 제조된 철 분말

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See also references of EP3878580A4

Also Published As

Publication number Publication date
KR102175428B1 (ko) 2020-11-06
JP2022506098A (ja) 2022-01-17
US20220008992A1 (en) 2022-01-13
KR20200051233A (ko) 2020-05-13
CN112969544A (zh) 2021-06-15
EP3878580A1 (fr) 2021-09-15
EP3878580A4 (fr) 2021-12-29

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