CN112969544A - Method for preparing needle-shaped or rod-shaped porous iron powder and needle-shaped or rod-shaped porous iron powder prepared by same - Google Patents

Method for preparing needle-shaped or rod-shaped porous iron powder and needle-shaped or rod-shaped porous iron powder prepared by same Download PDF

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Publication number
CN112969544A
CN112969544A CN201980072505.XA CN201980072505A CN112969544A CN 112969544 A CN112969544 A CN 112969544A CN 201980072505 A CN201980072505 A CN 201980072505A CN 112969544 A CN112969544 A CN 112969544A
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rod
ferrous chloride
iron powder
shaped
needle
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CN201980072505.XA
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Chinese (zh)
Inventor
韩吉秀
严炯燮
朴振均
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Research Institute of Industrial Science and Technology RIST
Posco Holdings Inc
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Posco Co Ltd
Research Institute of Industrial Science and Technology RIST
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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
    • B22F9/24—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
    • 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
    • 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

Abstract

The invention relates to a method for preparing needle-shaped or rod-shaped porous iron powder, and particularly provides a method for preparing needle-shaped or rod-shaped porous iron powder and the needle-shaped or rod-shaped porous iron powder prepared by the preparation method, wherein the method comprises the following steps: a step of concentrating the ferrous chloride aqueous solution to prepare ferrous chloride dihydrate; a step of performing solid-liquid separation on the ferrous chloride dihydrate to prepare ferrous chloride dihydrate powder; a step of oxidizing the ferrous chloride dihydrate powder; and reducing the oxidized ferrous chloride dihydrate.

Description

Method for preparing needle-shaped or rod-shaped porous iron powder and needle-shaped or rod-shaped porous iron powder prepared by same
Technical Field
The invention provides a method for preparing needle-shaped or rod-shaped porous iron powder and the needle-shaped or rod-shaped porous iron powder prepared by the method. More particularly, the present invention provides a method for preparing needle-shaped or rod-shaped porous iron powder using an aqueous solution of ferrous chloride and the needle-shaped or rod-shaped porous iron powder prepared thereby.
Background
The existing methods for preparing iron powder include a sponge-iron process (hot-reduction process) and a water-atomization process (water-atomization process). The sponge iron process is a process for reducing iron oxide to prepare porous iron powder. The water atomization process is a process of atomizing (atomizing) molten iron using high-pressure water spray, and the prepared iron powder is high-density (dense) powder and is not porous powder. In addition, the powder thus prepared is mostly angular, square, spherical or non-uniform in shape.
The iron oxide used in the sponge iron process can be iron ore or powder generated in an iron making process, iron oxide prepared by using acid-washing liquid generated after surface acid washing in an iron plate preparation process and the like as raw materials, and the porous iron powder prepared by the sponge iron process has the characteristics of wide specific surface area, high reactivity and strong reducibility, so that the porous iron powder can be used for self-lubricating bearing (self-lubricating bearings) materials; soil, groundwater, industrial wastewater purification materials (catalysts, reducing agents, etc.); a welding rod coating material; hand warmer material; an oxygen scavenger; raw materials for the production of iron compounds; extractants for cementation, and the like.
On the other hand, U.S. laid-open patent No. 2016-.
Disclosure of Invention
Technical problem
An aspect of the present invention is directed to a method for preparing an iron powder having needle-like or rod-like shape characteristics and porous characteristics.
Another aspect of the present invention is directed to an iron powder prepared by the preparation method according to the present invention.
Technical scheme
The invention provides a preparation method of needle-shaped or rod-shaped porous iron powder, which comprises the following steps: a step of concentrating the ferrous chloride aqueous solution to prepare ferrous chloride dihydrate; a step of performing solid-liquid separation on the ferrous chloride dihydrate to prepare ferrous chloride dihydrate powder; a step of oxidizing the ferrous chloride dihydrate powder; and reducing the oxidized ferrous chloride dihydrate.
Another aspect of the present invention provides a needle-shaped or rod-shaped porous iron powder prepared by the preparation method.
Effects of the invention
According to the process of the present invention, iron powder can be mass-produced from an iron chloride aqueous solution, and the iron powder thus produced has a porous needle-like or rod-like shape, and thus can be used not only in the field of conventional porous iron powder applications, but also to achieve the effects of improving the filling ratio, the workability, the physical properties, and the like, based on the rod-like powder characteristics.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the needle-shaped or rod-shaped porous iron powder of the present invention.
Fig. 2 shows SEM images of ferrous chloride dihydrate and ferrous chloride tetrahydrate crystals appearing when an aqueous ferrous chloride solution according to an embodiment of the present invention was concentrated.
Fig. 3 shows an image of an iron oxide powder obtained after a roasting process is performed on ferrous chloride dihydrate obtained by concentration of an aqueous ferrous chloride solution according to an embodiment of the present invention, taken by SEM.
Fig. 4 illustrates an image of reduced iron powder obtained after a reduction reaction of iron oxide powder according to an example of the present invention is taken by SEM.
Detailed Description
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention may be modified into various different forms, and the scope of the present invention is not limited to the embodiments described below.
The present invention is directed to a method for preparing an iron powder having needle-like or rod-like shape characteristics and porous characteristics and an iron powder prepared by the same.
Specifically, the preparation method of the needle-shaped or rod-shaped porous iron powder comprises the following steps: a step of concentrating the ferrous chloride aqueous solution to prepare ferrous chloride dihydrate; a step of performing solid-liquid separation on the ferrous chloride dihydrate to prepare ferrous chloride dihydrate powder; a step of oxidizing the ferrous chloride dihydrate powder; and reducing the oxidized ferrous chloride dihydrate.
The raw material of the ferrous chloride aqueous solution may be a post-solution generated after an acid washing process for removing oxides on the surface in an iron plate preparation process, a post-solution generated in other processes, or an aqueous solution in which iron is dissolved in hydrochloric acid, and the ferrous chloride aqueous solution is preferably an aqueous solution that is not saturated or supersaturated.
The concentration of the ferrous chloride aqueous solution is 20 to 625g/L, preferably 250 to 600 g/L. If the concentration is less than 20g/L, the energy for evaporating water during concentration is excessively consumed due to the small amount of ferrous chloride in the aqueous solution, and there is a problem that the amount of precipitated ferrous chloride dihydrate is small, whereas if it is more than 625g/L, the aqueous ferrous chloride solution is saturated or supersaturated, and precipitation occurs during transportation.
The step of preparing ferrous chloride dihydrate is to concentrate the aqueous ferrous chloride solution to precipitate supersaturated ferrous chloride dihydrate, in which case it may be concentrated, for example, by concentration by evaporation.
On the other hand, as for the solid-liquid separation performed in the step of producing ferrous chloride dihydrate powder, the precipitated ferrous chloride dihydrate may be separated by, for example, a centrifugal separator, but is not limited thereto, and the solid-liquid separation may be performed by any method that can be used for solid-liquid separation in the technical field, such as filtration or the like.
When the step of preparing ferrous chloride dihydrate is carried out by evaporative concentration, the temperature of the concentration process must be adjusted. At this time, for the evaporation concentration, for example, it is preferably carried out at a temperature of 72 to 125 ℃, more preferably at a temperature of 75 to 95 ℃. If the reaction is carried out at a temperature lower than 72 ℃, ferrous chloride tetrahydrate may be precipitated, which is problematic in that it precipitates in the form of a polygonal body having edges, whereas if the reaction is carried out at a temperature higher than 125 ℃, not only ferric chloride monohydrate but also excessive energy consumption may be caused. Fig. 2 shows an image of the precipitated angular polyhedron-shaped ferrous chloride tetrahydrate by SEM.
The step of oxidizing the ferrous chloride dihydrate powder may be performed by a roasting process of a pyrolysis reaction in an oxygen atmosphere. In the roasting process, ferrous chloride dihydrate reacts with oxygen as follows.
2(FeCl2H2O)+1/2O2→Fe2O3+4HCl(g)
In this case, not only Fe is produced by the reaction as described above2O3And also rare generation of Fe3O4Or an oxide of FeO.
In addition, the baking process may use, but is not limited to, a fluidized furnace, a rotary kiln (rotary kiln), a belt furnace, a drop tube furnace, or other reaction furnaces, and it is necessary to keep the rod-like shape by avoiding as much as possible the powder from being crushed due to external force acting on the powder during the reaction.
Further, the reaction of the firing process may be performed at a temperature of 200 to 1300 ℃. This is because, if the temperature is lower than 200 ℃, iron oxide is not generated, and if the temperature is higher than 1300 ℃, it is difficult to obtain iron oxide of a desired shape because of occurrence of iron oxide sintering. Preferably at a temperature of from 500 to 800 ℃.
In order to distinguish the shape of the iron oxide generated by the roasting process, classification may be performed. Further, the hydrochloric acid generated in the process is collected by a wet method to prepare an aqueous hydrochloric acid solution, and the aqueous hydrochloric acid solution can be used for preparing an aqueous ferrous chloride solution.
The step of reducing the oxidized ferrous chloride dihydrate may be performed by a reduction reaction of the oxidized ferrous chloride dihydrate under a high-temperature reducing atmosphere. In this case, the reducing atmosphere may be, for example, an atmosphere of hydrogen, carbon monoxide, or a mixture thereof, and a compound which can be converted into hydrogen, carbon monoxide, or a mixture thereof by a reaction such as decomposition may be used as the reducing agent. For example, the reduction reaction is as follows.
Fe2O3+3H2(g) Or 3CO (g) → 2Fe +3H2O (g) or 3CO2(g)
In this case, Fe rarely produced in the oxidation step3O4Or the FeO oxide is reduced by the following reaction.
FeO+H2(g) Or CO (g) → Fe + H2O (g) or CO2(g)
Fe3O4+4H2(g) Or 4CO (g) → 3Fe +4H2O (g) or 4CO2(g)
The reduction reaction may be performed using, but not limited to, a fluidized furnace, a rotary kiln (rotary kiln), a belt furnace, a drop tube furnace, or other reaction furnaces, and it is necessary to keep the rod-like shape by avoiding the powder from being crushed due to external force acting on the powder during the reaction as much as possible.
Further, the reduction reaction may be performed at a temperature of 400 to 1300 ℃. This is because, at a temperature lower than 400 ℃, the reaction rate is slow and the productivity is lowered, and at a temperature higher than 1300 ℃, the produced reduced iron is excessively sintered or the reduced iron fine structure is coarsened, and the porous structure is lost. When the reducing atmosphere is a hydrogen atmosphere, the reduction reaction may preferably be performed at a temperature of 600 to 800 ℃, and when the reducing atmosphere is a carbon monoxide atmosphere, the reduction reaction may preferably be performed at a temperature of 700 to 1000 ℃.
In order to distinguish the shape of the reduced iron produced by the reduction reaction, classification may be performed. Further, with respect to the reduced iron produced, reoxidation may occur due to good reactivity, and therefore the powder must be collected under an inert atmosphere.
The specific surface area of the needle-shaped or rod-shaped porous iron powder prepared by the preparation method is 0.3-3 m2A/g, preferably from 0.5 to 2.5m2(ii) in terms of/g. If the specific surface area of the iron powder is less than 0.3m2There is a problem that reactivity is low if it is larger than 3m2The solid content of the solid content is not particularly limited, and it may be any solid content.
Hereinafter, the present invention will be described in further detail by way of specific examples. The following embodiments are merely examples to facilitate understanding of the present invention, and the scope of the present invention is not limited to the following embodiments.
Modes for carrying out the invention
Examples
Utilizing ferrous chloride (FeCl) produced in a nickel hydrometallurgical process2) The aqueous solution is used to prepare needle-shaped or rod-shaped iron powder. An exemplary process is shown in fig. 1, with the specific process as follows.
The aqueous solution of ferrous chloride (220 g/L) was concentrated to make supersaturated ferrous chloride dihydrate (FeCl)2·2H2O) is precipitated. And carrying out solid-liquid separation on the precipitated ferrous chloride dihydrate by a centrifugal separation method to separate ferrous chloride dihydrate powder. At this time, the aqueous solution was concentrated at a temperature of 80 ℃.
An image of the ferrous chloride dihydrate crystal prepared in the step is shown in fig. 2 by SEM.
Next, the ferrous chloride dihydrate powder is charged into a rotary kiln and calcined by a pyrolysis reaction in a high-temperature atmosphere containing oxygen. Thus preparing needle-shaped or rod-shaped iron oxide.
The roasting process is carried out at 700 c for 90 minutes and classification is carried out to distinguish the shape of the needle-like or rod-like iron oxide produced. Further, not only the Fe is generated2O3Fe may also be rarely produced3O4Or an oxide of FeO. On the other hand, HCl produced together in the rotary furnace is collected with a scrubber (scrubber) for reuse in the nickel smelting process.
An image of the iron oxide powder produced by the process as described above taken by SEM is shown in fig. 3.
Next, the needle-shaped or rod-shaped iron oxide is injected into a mesh belt type (mesh belt) furnace, and reduced iron powder is prepared by a reduction reaction under a high-temperature gas reducing atmosphere. In this case, the gas reducing atmosphere is a hydrogen or carbon monoxide atmosphere.
The reduction reaction is performed at 750 ℃ for 60 minutes, and classification is performed to distinguish the shape of the produced needle-shaped or rod-shaped iron oxide, thereby distinguishing needle-shaped or rod-shaped reduced iron powder from fine reduced iron powder.
The resultant needle-like or rod-like reduced iron powder was a powder having a length of about 500 μm and an aspect ratio (aspect ratio) of about 5, and a specific surface area of about 2.3m2(ii) in terms of/g. At this time, the produced reduced iron has good reactivity and is likely to undergo reoxidation, so that it is necessary to collect the powder under an inert atmosphere.
An image of a fine reduced iron produced by the process as described above taken by SEM is shown in fig. 4.
In the foregoing, the embodiments of the present invention have been described in detail, but the scope of the right of the present invention is not limited to the above-described embodiments, and it will be apparent to those of ordinary skill in the art that various modifications and variations can be made within the scope not departing from the technical idea of the present invention described in the claims.

Claims (10)

1. A method for preparing needle-shaped or rod-shaped porous iron powder, which comprises the following steps:
a step of concentrating the ferrous chloride aqueous solution to prepare ferrous chloride dihydrate;
a step of performing solid-liquid separation on the ferrous chloride dihydrate to prepare ferrous chloride dihydrate powder;
a step of oxidizing the ferrous chloride dihydrate powder; and
and (3) reducing the oxidized ferrous chloride dihydrate.
2. The method for preparing needle-like or rod-like porous iron powder according to claim 1, wherein,
the concentration of the ferrous chloride aqueous solution is 20 to 625 g/L.
3. The method for preparing needle-like or rod-like porous iron powder according to claim 1, wherein,
the concentration of the aqueous ferrous chloride solution is carried out by concentration by evaporation at a temperature of 72 to 125 ℃.
4. The method for preparing needle-like or rod-like porous iron powder according to claim 1, wherein,
the step of oxidizing the ferrous chloride dihydrate powder is carried out by calcination at a temperature of 200 to 1300 ℃ under an oxygen atmosphere.
5. The method for preparing needle-like or rod-like porous iron powder according to claim 1, wherein,
the step of reducing the ferrous chloride dihydrate powder is carried out at a temperature of 400 to 1300 ℃ in a reducing atmosphere.
6. The method for preparing needle-like or rod-like porous iron powder according to claim 5, wherein,
the reducing atmosphere is hydrogen, carbon monoxide or a mixed gas atmosphere thereof.
7. The method for preparing needle-like or rod-like porous iron powder according to claim 6, wherein,
the step of reducing the ferrous chloride dihydrate powder is carried out at a temperature of 600 to 800 ℃ under a hydrogen atmosphere.
8. The method for preparing needle-like or rod-like porous iron powder according to claim 6, wherein,
the step of reducing the ferrous chloride dihydrate powder is carried out at a temperature of 700 to 1000 ℃ under a carbon monoxide atmosphere.
9. A needle-like or rod-like porous iron powder prepared by the preparation method according to any one of claims 1 to 8.
10. The needle-like or rod-like porous iron powder according to claim 9, wherein,
the specific surface area of the iron powder is 0.3 to 3m2/g。
CN201980072505.XA 2018-11-05 2019-11-04 Method for preparing needle-shaped or rod-shaped porous iron powder and needle-shaped or rod-shaped porous iron powder prepared by same Withdrawn CN112969544A (en)

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KR1020180134325A KR102175428B1 (en) 2018-11-05 2018-11-05 Manufacturing method of cylindrical porous iron powder
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PCT/KR2019/014795 WO2020096293A1 (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

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GB662051A (en) * 1948-01-06 1951-11-28 Davide Primavesi Improved chemical process for producing powdered iron
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CN101898800A (en) * 2010-02-03 2010-12-01 深圳市东江环保股份有限公司 Method for preparing iron oxide red by using ferrous chloride
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KR20170076853A (en) * 2015-12-24 2017-07-05 주식회사 포스코 Method for manufacturing iron oxide

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