JP2015025164A - Method of producing agglomerate - Google Patents

Method of producing agglomerate Download PDF

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JP2015025164A
JP2015025164A JP2013154793A JP2013154793A JP2015025164A JP 2015025164 A JP2015025164 A JP 2015025164A JP 2013154793 A JP2013154793 A JP 2013154793A JP 2013154793 A JP2013154793 A JP 2013154793A JP 2015025164 A JP2015025164 A JP 2015025164A
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heat
agglomerate
powder
iron oxide
particle size
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JP5827648B2 (en
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脩 土屋
Osamu Tsuchiya
脩 土屋
田中 英年
Hidetoshi Tanaka
英年 田中
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Kobe Steel Ltd
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Kobe Steel Ltd
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Priority to AU2014294413A priority patent/AU2014294413B2/en
Priority to CN201480041173.6A priority patent/CN105452496A/en
Priority to PCT/JP2014/063829 priority patent/WO2015011981A1/en
Priority to EP14829405.1A priority patent/EP3026129A4/en
Priority to RU2016102002A priority patent/RU2638487C2/en
Priority to US14/908,055 priority patent/US20160168654A1/en
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • C21B13/14Multi-stage processes processes carried out in different vessels or furnaces
    • C21B13/146Multi-step reduction without melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/14Agglomerating; Briquetting; Binding; Granulating
    • C22B1/16Sintering; Agglomerating
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • C21B13/0046Making spongy iron or liquid steel, by direct processes making metallised agglomerates or iron oxide
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • C21B13/0066Preliminary conditioning of the solid carbonaceous reductant
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/14Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24Binding; Briquetting ; Granulating
    • C22B1/2406Binding; Briquetting ; Granulating pelletizing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/14Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24Binding; Briquetting ; Granulating

Abstract

PROBLEM TO BE SOLVED: To provide a method of producing an agglomerate by granulating a fine powder containing iron oxide, more specifically a powder containing iron oxide having a 50% particle size of 2 μm or smaller, so that the powder containing iron oxide is available as a raw material for iron production and a technique of producing reduced iron from an agglomerate obtained by agglomeration.SOLUTION: A method of producing an agglomerate includes a step of heat-treating a powder containing iron oxide having a 50% particle size of 2 μm or smaller at a heating temperature of 900-1,200°C and a step of producing an agglomerate by granulating with the obtained heat-treated powder as the raw material.

Description

本発明は、50%粒子径が2μm以下の微細な酸化鉄含有粉末を鉄源として有効利用する技術に関するものである。   The present invention relates to a technique for effectively using a fine iron oxide-containing powder having a 50% particle size of 2 μm or less as an iron source.

鉄鉱石等の酸化鉄含有物質から還元鉄を製造する方法としては、例えば、天然ガスを利用したガス還元法が知られている。近年開発された還元鉄の製造方法としては、酸化鉄含有物質と、炭材等の炭素質還元剤を混合した塊成物を、1300℃以上の高温で加熱して還元塊成物を製造するFASTMET法や、該還元塊成物を更に加熱してスラグと溶融分離し、粒状還元鉄を製造するITmk3法がある。   As a method for producing reduced iron from an iron oxide-containing substance such as iron ore, for example, a gas reduction method using natural gas is known. As a method for producing reduced iron developed in recent years, an agglomerate obtained by mixing an iron oxide-containing substance and a carbonaceous reducing agent such as a carbonaceous material is heated at a high temperature of 1300 ° C. or more to produce a reduced agglomerate. There are a FASTMET method and an ITmk3 method in which the reduced agglomerate is further heated and melted and separated from slag to produce granular reduced iron.

このように酸化鉄含有物質から還元鉄を製造するにあたっては、酸化鉄含有物質を原料として水やバインダーをミキサー内で混合し、造粒機で造粒してφ13〜18mmの塊成物としたものが用いられる。   Thus, in producing reduced iron from an iron oxide-containing substance, water and a binder are mixed in a mixer using the iron oxide-containing substance as a raw material, and granulated by a granulator to obtain an agglomerate having a diameter of 13 to 18 mm. Things are used.

粉末の塊成化法としては、例えば、ペレタイジング法や焼結法が知られており、粉末の粒度範囲に応じて事前処理としての適切な造粒方法が定められている(例えば、非特許文献1)。具体的には、ペレタイジング法に於ける転動造粒法では、50%粒子径が4μm以上であることが推奨され、焼結法では、50%粒子径が約0.11mm〜約3mm程度であることが推奨されている。   As the agglomeration method of the powder, for example, a pelletizing method and a sintering method are known, and an appropriate granulation method as a pretreatment is determined according to the particle size range of the powder (for example, non-patent document). 1). Specifically, in the rolling granulation method in the pelletizing method, it is recommended that the 50% particle size is 4 μm or more, and in the sintering method, the 50% particle size is about 0.11 mm to about 3 mm. It is recommended that there be.

ところで、鉄以外の有価金属には、NiやAl、Tiなどがある。これらの有価金属は、Ni含有鉱石やAl含有鉱石(赤泥)、Ti含有鉱石(イルメナイト)などからNi、Al、Tiを分離回収している。   By the way, valuable metals other than iron include Ni, Al, Ti and the like. These valuable metals separate and recover Ni, Al, and Ti from Ni-containing ore, Al-containing ore (red mud), Ti-containing ore (ilmenite), and the like.

例えば、Ni含有鉱石からNiを分離回収する方法としては、HPAL法(High Pressure Acid Leach。高圧硫酸浸出)が知られている。この方法では、Ni含有鉱石を高温高圧状態の硫酸と安定的に反応させることによりNiを抽出回収できる。Niを抽出回収した後には、沈降分離産物(残渣)が生成する。この残渣には、酸化鉄(主にヘマタイト。Fe23)が多く含まれている。また、この残渣に含まれる水分量は20%以上で、その形態は泥状で、50%粒子径は約0.6μmと非常に微細である。 For example, the HPAL method (High Pressure Acid Leach) is known as a method for separating and recovering Ni from Ni-containing ores. In this method, Ni can be extracted and recovered by stably reacting Ni-containing ore with sulfuric acid in a high-temperature and high-pressure state. After extracting and recovering Ni, a sedimentation product (residue) is generated. This residue is rich in iron oxide (mainly hematite, Fe 2 O 3 ). Further, the amount of water contained in the residue is 20% or more, the form is mud, and the 50% particle size is very fine as about 0.6 μm.

「鉄と鋼」、鉱石の磨鉱特性とペレタイジング適正粒度の関係について、日本鉄鋼協会会誌、第49年(1963)、第3号、P.346〜348Regarding the relationship between “Iron and Steel”, ore grinding characteristics and pelletizing appropriate particle size, Journal of the Japan Iron and Steel Institute, 49th (1963), No. 3, p. 346-348

選鉱操作で目的成分を回収した残渣(以下、尾鉱ということがある。)には、上述したように、酸化鉄(例えば、ヘマタイト)が多く含まれていることがある。そのため尾鉱に含まれる酸化鉄を還元して鉄源として利用することが考えられる。しかし、尾鉱は、通常、非常に微細になっているため、上記の転動造粒法で造粒し、製鉄原料として用いることは困難である。即ち、粒子が非常に細かい場合には、混合機内における攪拌過程で粒子が相互に容易に粘着し、粒子が擬似粒子を形成する。この擬似粒子を造粒機で造粒すると、擬似粒子同士が結合して成長し、金平糖状のペレットが形成される。このような形状のペレットは、内部の組織が不均一となっており、また強度が低いため、製鉄原料として用いることはできない。従って尾鉱を塊成化して製鉄原料として用い、鉄源として有効利用することは難しい。   As described above, the residue obtained by collecting the target component by the beneficiation operation (hereinafter sometimes referred to as tailing) may contain a large amount of iron oxide (for example, hematite). Therefore, it is conceivable to reduce the iron oxide contained in the tailings and use it as an iron source. However, since tailings are usually very fine, it is difficult to granulate by the tumbling granulation method described above and use it as an iron-making raw material. That is, when the particles are very fine, the particles easily stick to each other during the stirring process in the mixer, and the particles form pseudo particles. When the pseudo particles are granulated by a granulator, the pseudo particles are bonded to each other and grow to form a confetti pellet. The pellet having such a shape cannot be used as an iron-making raw material because the internal structure is not uniform and the strength is low. Therefore, it is difficult to agglomerate tailings and use it as a raw material for iron making and effectively use it as an iron source.

本発明は上記の様な事情に着目してなされたものであって、その目的は、微細な酸化鉄含有粉末(具体的には、50%粒子径が2μm以下の酸化鉄含有粉末)を製鉄原料として利用できるように造粒して塊成物を製造する方法を提供することにある。また、本発明の他の目的は、塊成化して得られた塊成物から還元鉄を製造する技術を提供することにある。   The present invention has been made paying attention to the above-mentioned circumstances, and the object thereof is to produce fine iron oxide-containing powder (specifically, iron oxide-containing powder having a 50% particle diameter of 2 μm or less). The object is to provide a method for producing an agglomerate by granulation so that it can be used as a raw material. Another object of the present invention is to provide a technique for producing reduced iron from an agglomerate obtained by agglomeration.

本発明者らは、微細な酸化鉄含有粉末を造粒して塊成化し、製鉄原料として用いるために鋭意検討を重ねてきた。その結果、50%粒子径が2μm以下の酸化鉄含有粉末を所定の温度で熱処理すれば、粒子が相互に焼結して粗大化するため造粒可能となり、塊成物を製造できることを見出し、本発明を完成した。   The inventors of the present invention have made extensive studies in order to granulate and agglomerate fine iron oxide-containing powder and use it as an iron-making raw material. As a result, it was found that if the iron oxide-containing powder having a 50% particle size of 2 μm or less is heat-treated at a predetermined temperature, the particles can be granulated because they are sintered together and coarsened, and an agglomerate can be produced. The present invention has been completed.

即ち、上記課題を解決できた本発明に係る塊成物の製造方法とは、50%粒子径が2μm以下の酸化鉄含有粉末を、加熱温度900〜1200℃で熱処理する工程と、得られた熱処理粉末を造粒して塊成物を製造する工程と、を含む点に要旨を有している。   That is, the method for producing an agglomerate according to the present invention, which was able to solve the above problems, was obtained by heat-treating an iron oxide-containing powder having a 50% particle diameter of 2 μm or less at a heating temperature of 900 to 1200 ° C. And a step of producing an agglomerate by granulating the heat-treated powder.

前記造粒は、転動造粒法によって行えばよい。   The granulation may be performed by a rolling granulation method.

前記熱処理は、前記熱処理粉末の50%粒子径が4μm以上となるように行うことが好ましく、加熱時間は、例えば、30分以上とすればよい。前記熱処理は、前記酸化鉄含有粉末を転動させつつ行うことが好ましい。   The heat treatment is preferably performed so that the 50% particle diameter of the heat treated powder is 4 μm or more, and the heating time may be, for example, 30 minutes or more. The heat treatment is preferably performed while rolling the iron oxide-containing powder.

前記酸化鉄含有粉末としては、尾鉱を用いることができる。前記尾鉱としては、例えば、Ni含有鉱石からNiを回収した後の残渣を用いることができる。   As the iron oxide-containing powder, tailings can be used. As the tailing, for example, a residue after recovering Ni from Ni-containing ore can be used.

本発明には、上記の製造方法で得られた塊成物を原料とし、これを加熱して酸化鉄を還元し、還元鉄を製造する方法も包含される。前記塊成物には、例えば、炭素質還元剤を更に含んでもよい。   The present invention also includes a method of producing reduced iron by using the agglomerate obtained by the above production method as a raw material and heating it to reduce iron oxide. The agglomerate may further contain, for example, a carbonaceous reducing agent.

本発明によれば、50%粒子径が2μm以下の酸化鉄含有粉末を、加熱温度900〜1200℃で熱処理することによって、粒子を粗大化できるため、従来の方法で造粒でき、球状の塊成物を製造できる。得られた塊成物は、製鉄原料として利用できる。   According to the present invention, the iron oxide-containing powder having a 50% particle diameter of 2 μm or less is heat-treated at a heating temperature of 900 to 1200 ° C., whereby the particles can be coarsened. The composition can be manufactured. The obtained agglomerate can be used as a raw material for iron making.

図1は、加熱温度400℃で熱処理して得られた熱処理粉末を撮影した図面代用写真である。FIG. 1 is a drawing-substituting photograph in which a heat-treated powder obtained by heat treatment at a heating temperature of 400 ° C. is photographed. 図2は、加熱温度1200℃で熱処理して得られた熱処理粉末を撮影した図面代用写真である。FIG. 2 is a drawing-substituting photograph in which a heat-treated powder obtained by heat treatment at a heating temperature of 1200 ° C. is photographed. 図3は、熱処理粉末の粒度分布を示すグラフである。FIG. 3 is a graph showing the particle size distribution of the heat-treated powder. 図4は、加熱温度400℃で熱処理して得られた熱処理粉末をボールミルで解砕した後、造粒した塊成物を撮影した図面代用写真である。FIG. 4 is a drawing-substituting photograph in which an agglomerated product obtained by granulating a heat-treated powder obtained by heat treatment at a heating temperature of 400 ° C. with a ball mill is photographed. 図5は、加熱温度1200℃で熱処理して得られた熱処理粉末をボールミルで粉砕した後、造粒した塊成物を撮影した図面代用写真である。FIG. 5 is a drawing-substituting photograph in which an agglomerated product obtained by granulating a heat-treated powder obtained by heat-treating at a heating temperature of 1200 ° C. with a ball mill is photographed.

本発明法は、
50%粒子径が2μm以下の酸化鉄含有粉末を、加熱温度900〜1200℃で熱処理する工程(以下、熱処理工程ということがある)と、
得られた熱処理粉末を原料として造粒して塊成物を製造する工程(以下、塊成化工程ということがある)と、
を含むものである。以下、各工程に沿って詳細に説明する。
The method of the present invention
A step of heat-treating an iron oxide-containing powder having a 50% particle diameter of 2 μm or less at a heating temperature of 900 to 1200 ° C. (hereinafter sometimes referred to as a heat treatment step)
A step of granulating the obtained heat-treated powder as a raw material to produce an agglomerate (hereinafter sometimes referred to as an agglomeration step);
Is included. Hereinafter, it demonstrates in detail along each process.

[熱処理工程]
本発明法では、50%粒子径が2μm以下の酸化鉄含有粉末を用いることを前提としており、こうした微細な酸化鉄粉末を造粒して塊成化し、鉄源として有効活用することを目的としている。
[Heat treatment process]
In the method of the present invention, it is premised that an iron oxide-containing powder having a 50% particle diameter of 2 μm or less is used. For the purpose of granulating and agglomerating such fine iron oxide powder, it can be effectively used as an iron source. Yes.

上記50%粒子径が2μm以下の酸化鉄含有粉末としては、尾鉱を用いることができる。   As the iron oxide-containing powder having a 50% particle diameter of 2 μm or less, tailing can be used.

上記尾鉱とは、選鉱操作で目的成分を回収した残渣を意味し、選鉱前の鉱物の種類は特に限定されない。尾鉱としては、例えば、鉄鉱石からの選鉱後の残渣、Al含有鉱石からAlを回収した後の残渣、Ti含有鉱石からTiを回収した後の残渣、Ni含有鉱石からNiを回収した後の残渣、などを用いることができる。   The tailing means a residue obtained by recovering the target component by the beneficiation operation, and the type of mineral before the beneficiation is not particularly limited. As tailings, for example, residues after beneficiation from iron ore, residues after recovering Al from Al-containing ores, residues after recovering Ti from Ti-containing ores, and after recovering Ni from Ni-containing ores Residues, etc. can be used.

Al含有鉱石としては赤泥、Ti含有鉱石としてはイルメナイト、Ni含有鉱石としてはサプロライトなどが用いられている。例えば、Ni含有鉱石からNiを回収する方法としては、上述したHPAL法が知られており、Niを分離回収したあとの残渣は、50%粒子径が2μm以下となる。   Red mud is used as the Al-containing ore, ilmenite is used as the Ti-containing ore, and saprolite is used as the Ni-containing ore. For example, as a method for recovering Ni from Ni-containing ore, the above-described HPAL method is known, and the residue after separating and recovering Ni has a 50% particle size of 2 μm or less.

上記熱処理工程では、上記50%粒子径が2μm以下の酸化鉄含有粉末を、加熱温度900〜1200℃で熱処理する。この温度域で微細な酸化鉄含有粉末を熱処理することによって、酸化鉄含有粉末は酸化し、焼結して粗大化する。その結果、後記の工程で造粒可能な大きさに成長させることができる。   In the heat treatment step, the iron oxide-containing powder having a 50% particle size of 2 μm or less is heat-treated at a heating temperature of 900 to 1200 ° C. By heat-treating the fine iron oxide-containing powder in this temperature range, the iron oxide-containing powder is oxidized, sintered, and coarsened. As a result, it can be grown to a size that allows granulation in the steps described below.

上記加熱温度が900℃を下回ると、粗大化効果が得られず、造粒できないか、造粒できたとしても球状の塊成物は得られない。従って加熱温度は900℃以上とし、好ましくは950℃以上、より好ましくは1000℃以上とする。しかし加熱温度が1200℃を超えると、粗大な塊成物を形成したり、塊成物が熱処理装置の表面に付着するという問題が生じる。従って加熱温度は1200℃以下とし、好ましくは1150℃以下、より好ましくは1100℃以下とする。   When the heating temperature is lower than 900 ° C., the effect of coarsening cannot be obtained, and granulation cannot be performed or even if granulation can be performed, a spherical agglomerate cannot be obtained. Therefore, the heating temperature is 900 ° C. or higher, preferably 950 ° C. or higher, more preferably 1000 ° C. or higher. However, when heating temperature exceeds 1200 degreeC, the problem that a coarse agglomerate will be formed or an agglomerate will adhere to the surface of a heat processing apparatus will arise. Therefore, the heating temperature is 1200 ° C. or lower, preferably 1150 ° C. or lower, more preferably 1100 ° C. or lower.

上記加熱温度は、炉内に熱電対を差し込み、炉の中央部における雰囲気温度を測定してこの温度に基づいて制御すればよい。   The heating temperature may be controlled based on this temperature by inserting a thermocouple into the furnace and measuring the ambient temperature in the center of the furnace.

上記熱処理は、上記熱処理粉末の50%粒子径が4μm以上となるように、上記加熱温度を考慮して加熱時間を制御すればよい。   In the heat treatment, the heating time may be controlled in consideration of the heating temperature so that the 50% particle diameter of the heat treated powder is 4 μm or more.

上記加熱時間は、例えば、30分間以上とすることが好ましい。加熱時間は、より好ましくは40分間以上であり、更に好ましくは50分間以上である。加熱時間の上限は特に限定されないが、加熱時間を長くしても粒子径粗大化効果は飽和する反面、生産性が低下するため、例えば、60分間以下とすればよい。   The heating time is preferably 30 minutes or longer, for example. The heating time is more preferably 40 minutes or more, and further preferably 50 minutes or more. The upper limit of the heating time is not particularly limited, but even if the heating time is lengthened, the effect of coarsening the particle diameter is saturated, but the productivity is lowered. For example, the heating time may be 60 minutes or less.

上記熱処理は、酸化性雰囲気下で行えばよく、例えば、大気雰囲気で行えばよい。   The heat treatment may be performed in an oxidizing atmosphere, for example, in an air atmosphere.

上記熱処理は、上記酸化鉄含有粉末を均一に加熱するために、転動させつつ行うことが好ましい。上記加熱炉としては、回転式加熱炉を用いればよい。   The heat treatment is preferably performed while rolling in order to uniformly heat the iron oxide-containing powder. A rotary heating furnace may be used as the heating furnace.

上記回転式加熱炉とは、加熱面(炉面)が回転軸を中心に回転している炉であり、この回転軸は水平以上、垂直未満になっている炉を意味する。   The rotary heating furnace is a furnace in which a heating surface (furnace surface) rotates around a rotation axis, and this rotation axis means a furnace that is at least horizontal and less than vertical.

[塊成化工程]
塊成化工程では、上記熱処理工程で得られた熱処理粉末を原料とし、造粒して塊成物を製造する。
[Agglomeration process]
In the agglomeration step, the heat treated powder obtained in the heat treatment step is used as a raw material, and granulated to produce an agglomerate.

上記熱処理粉末を造粒する方法としては、例えば、転動造粒法が挙げられる。   Examples of a method for granulating the heat treated powder include a rolling granulation method.

上記熱処理粉末は、塊成物の粒径が、例えば、10〜16mmとなるように造粒することが好ましい。   The heat-treated powder is preferably granulated so that the particle size of the agglomerate is, for example, 10 to 16 mm.

上記熱処理粉末は、造粒するに先立って、解砕または粉砕してもよい。解砕機または粉砕機としては公知のものを用いることができ、例えば、ボールミル、ローラミル、ロールクラッシャなどを用いることができる。   The heat-treated powder may be pulverized or pulverized prior to granulation. A well-known thing can be used as a crusher or a grinder, for example, a ball mill, a roller mill, a roll crusher etc. can be used.

[その他]
上記塊成化工程で得られた塊成物は、製鉄原料として用いることができる。例えば、得られた塊成物を加熱硬化処理後、高炉に投入したり、さらに加熱硬化物を還元性ガス雰囲気で加熱して酸化鉄を還元することによって、還元鉄を製造できる。
[Other]
The agglomerate obtained in the agglomeration process can be used as a raw material for iron making. For example, reduced iron can be produced by putting the obtained agglomerated material into a blast furnace after heat-curing treatment, or further heating the heat-cured material in a reducing gas atmosphere to reduce iron oxide.

また、上記熱処理粉末に、更に炭素質還元剤やバインダーなどを配合して塊成物とし、これを加熱炉内で加熱することによって、還元鉄を製造できる。   Moreover, a reduced iron can be manufactured by mix | blending a carbonaceous reducing agent, a binder, etc. with the said heat processing powder, and making it an agglomerate, and heating this in a heating furnace.

以上、本発明によれば、50%粒子径が2μm以下の酸化鉄含有粉末を所定の温度域で熱処理することによって造粒可能な粒子径に粗大化できるため、熱処理により得られた熱処理粉末を原料として造粒すれば、熱処理粉末が雪だるま状に成長した均一な組織構造の塊成物を製造できる。   As described above, according to the present invention, since the iron oxide-containing powder having a 50% particle size of 2 μm or less can be coarsened to a granulated particle size by heat treatment in a predetermined temperature range, When granulated as a raw material, an agglomerate having a uniform texture structure in which the heat-treated powder has grown into a snowman shape can be produced.

以下、実施例を挙げて本発明をより具体的に説明するが、本発明はもとより下記実施例によって制限を受けるものではなく、前・後記の趣旨に適合し得る範囲で適当に変更を加えて実施することも勿論可能であり、それらはいずれも本発明の技術的範囲に包含される。   EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited by the following examples, but may be appropriately modified within a range that can meet the purpose described above and below. Of course, it is possible to implement them, and they are all included in the technical scope of the present invention.

50%粒子径が2μm以下の酸化鉄含有粉末を熱処理し、得られた熱処理粉末を造粒して塊成物を製造した。   An iron oxide-containing powder having a 50% particle size of 2 μm or less was heat-treated, and the obtained heat-treated powder was granulated to produce an agglomerate.

上記50%粒子径が2μm以下の酸化鉄含有粉末としては、Ni含有鉱石からNiを回収した後の残渣(尾鉱。水分量は約27%)を屋外に放置して天日に曝し、水分量を約19%としたものを用いた。   As the iron oxide-containing powder having a 50% particle size of 2 μm or less, the residue (tail ore, water content is about 27%) after recovering Ni from the Ni-containing ore is left outdoors and exposed to the sun. An amount of about 19% was used.

Ni回収後の残渣の成分組成を下記表1に示す。下記表1において、LOIは、イグニションロス量(灼熱減量)を示す。   The component composition of the residue after Ni recovery is shown in Table 1 below. In Table 1 below, LOI represents the amount of ignition loss (loss of ignition).

水分量を約19%に調整した尾鉱は、赤褐色であり、これを回転加熱装置に2kg装入し、尾鉱を転動させつつ熱処理して乾燥および焼結させた。熱処理時の加熱温度は、下記表2に示すように、400℃、800℃、1100℃または1200℃とした。加熱時間は、下記表2に示すように、加熱温度が400℃の場合は約60分間、加熱温度が800℃、1100℃または1200℃の場合は約30分間とした。加熱雰囲気は空気流通下とした。   The tailing whose water content was adjusted to about 19% was reddish brown. This was charged in 2 kg into a rotary heating device, and heat-dried while rolling the tailing and dried and sintered. As shown in Table 2 below, the heating temperature during the heat treatment was set to 400 ° C., 800 ° C., 1100 ° C., or 1200 ° C. As shown in Table 2 below, the heating time was about 60 minutes when the heating temperature was 400 ° C, and about 30 minutes when the heating temperature was 800 ° C, 1100 ° C, or 1200 ° C. The heating atmosphere was under air circulation.

熱処理して得られた粉末は、加熱温度を400℃、800℃または1100℃とした場合は赤褐色のままであったが、加熱温度を1200℃とした場合は黒褐色に変化した。参考として、加熱温度を400℃として得られた粉末を撮影した図面代用写真を図1に示す。また、加熱温度を1200℃として得られた粉末を撮影した図面代用写真を図2に示す。   The powder obtained by the heat treatment remained reddish brown when the heating temperature was 400 ° C, 800 ° C or 1100 ° C, but changed to blackish brown when the heating temperature was 1200 ° C. For reference, FIG. 1 shows a drawing-substituting photograph in which the powder obtained at a heating temperature of 400 ° C. is photographed. Moreover, the drawing substitute photograph which image | photographed the powder obtained by heating temperature to 1200 degreeC is shown in FIG.

熱処理後、室温まで冷却した熱処理粉末をボールミルで解砕または粉砕し、これを造粒用試料とした。加熱温度を400℃、800℃または1100℃として得られた熱処理粉末については、ボールミルで約30秒間解砕し、加熱温度を1200℃として得られた熱処理粉末については、ボールミルで約20分間粉砕した。   After the heat treatment, the heat treated powder cooled to room temperature was pulverized or pulverized with a ball mill, and this was used as a granulation sample. The heat-treated powder obtained at a heating temperature of 400 ° C., 800 ° C. or 1100 ° C. was crushed by a ball mill for about 30 seconds, and the heat-treated powder obtained at a heating temperature of 1200 ° C. was crushed by a ball mill for about 20 minutes. .

各熱処理粉末の粒度分布を測定し、結果を図3に示す。図3の横軸は粒子径(μm)、縦軸は積算篩下質量(質量%)を示している。   The particle size distribution of each heat-treated powder was measured, and the results are shown in FIG. The horizontal axis in FIG. 3 indicates the particle diameter (μm), and the vertical axis indicates the total sieve mass (mass%).

また、50%粒子径(μm)、粒子径が1μm未満の積算篩下質量(質量%)、粒子径が10μm未満の積算篩下質量(質量%)を夫々算出し、下記表2に示す。   Further, 50% particle diameter (μm), integrated sieve mass (mass%) having a particle diameter of less than 1 μm, and integrated sieve mass (mass%) having a particle diameter of less than 10 μm are calculated and shown in Table 2 below.

図3および表2から明らかなように、加熱温度を400℃または800℃として熱処理して得られた粉末は、50%粒子径は熱処理前の原料粉末とほぼ同じであり、粒子径が1μm未満の積算篩下質量もほぼ同じであった。従って原料粉末、加熱温度を400℃または800℃として熱処理して得られた粉末は、粒子径はいずれも10μm未満であり、ほぼ同じ粒度構成であった。   As is clear from FIG. 3 and Table 2, the powder obtained by heat treatment at a heating temperature of 400 ° C. or 800 ° C. has a 50% particle size almost the same as the raw material powder before the heat treatment, and the particle size is less than 1 μm. The total sieve mass of was also almost the same. Therefore, the raw material powder and the powder obtained by heat treatment at a heating temperature of 400 ° C. or 800 ° C. all had a particle size of less than 10 μm and almost the same particle size constitution.

これに対し、加熱温度を1100℃として熱処理して得られた粉末は、50%粒子径は熱処理前の原料粉末よりも約8.6倍大きくなっており、熱処理によって粒子が粗粒化していることが分かる。   In contrast, the powder obtained by heat treatment at a heating temperature of 1100 ° C. has a 50% particle size that is approximately 8.6 times larger than the raw material powder before the heat treatment, and the particles are coarsened by the heat treatment. I understand that.

加熱温度を1200℃として熱処理して得られた粉末は、50%粒子径は熱処理前の原料粉末よりも約53.5倍大きくなっており、粒子径が1μm未満の積算篩下質量は4.4質量%にまで低減でき、熱処理によって粒子が粗粒化していることが分かる。   The powder obtained by heat treatment at a heating temperature of 1200 ° C. has a 50% particle size that is about 53.5 times larger than that of the raw material powder before the heat treatment, and the cumulative sieving mass with a particle size of less than 1 μm is 4. It can be reduced to 4% by mass, and it can be seen that the particles are coarsened by heat treatment.

粒子の粗粒化は、粒子径が1μm未満の積算篩下質量および粒子径が10μm未満の積算篩下質量の結果からも読み取れ、原料粉末や加熱温度を400℃または800℃としても、粒子径が10μm未満の粉末のみであったのに対し、加熱温度を1200℃として熱処理することによって、粒子径が10μm未満の粉末の割合は20.9%となり、粒子径が10μm以上の粗大な粉末の割合を約80%とすることができた。   The coarsening of the particles can also be read from the results of the cumulative sieving mass with a particle size of less than 1 μm and the cumulative sieving mass with a particle size of less than 10 μm. However, when the heat treatment was performed at a heating temperature of 1200 ° C., the proportion of the powder having a particle size of less than 10 μm was 20.9%, and the coarse powder having a particle size of 10 μm or more was used. The ratio could be about 80%.

次に、熱処理粉末の各粒度範囲別の粒度分布値に基づいて、粒子径を球状と仮定して比表面積(cm2/g)を計算によって求めた。結果を下記表2に示す。 Next, based on the particle size distribution value for each particle size range of the heat-treated powder, the specific surface area (cm 2 / g) was calculated by assuming that the particle diameter was spherical. The results are shown in Table 2 below.

下記表2から明らかなように、加熱温度を400℃または800℃として熱処理して得られた粉末の比表面積(計算値)は27400〜29380cm2/gであったのに対し、加熱温度を1100℃として熱処理して得られた粉末の比表面積(計算値)は8520cm2/g、加熱温度を1200℃として熱処理して得られた粉末の比表面積(計算値)は1920cm2/gであった。この結果から、加熱温度を高くするほど、比表面積は小さくなり、粒子が粗大化していることが分かる。 As is apparent from Table 2 below, the specific surface area (calculated value) of the powder obtained by heat treatment at a heating temperature of 400 ° C. or 800 ° C. was 27400 to 29380 cm 2 / g, whereas the heating temperature was 1100. The specific surface area (calculated value) of the powder obtained by heat treatment at 0 ° C. was 8520 cm 2 / g, and the specific surface area (calculated value) of the powder obtained by heat treatment at 1200 ° C. was 1920 cm 2 / g. . From this result, it can be seen that the higher the heating temperature, the smaller the specific surface area and the larger the particles.

次に、熱処理粉末を約φ35cmのゴムタイヤ製・造粒機に装入し、適量の水を加えて造粒した。その結果、加熱温度を400℃または800℃として得られた熱処理粉末のボールミル解砕物を用いた場合は、ペレットの形状は球状にはならず、金平糖のように表面に突起があるものとなった。加熱温度を400℃として得られた熱処理粉末の解砕物を用いて造粒した塊成物を撮影した図面代用写真を図4に示す。   Next, the heat-treated powder was placed in a rubber tire granulator with a diameter of about 35 cm and granulated by adding an appropriate amount of water. As a result, when a heat-treated powder ball mill pulverized product obtained at a heating temperature of 400 ° C. or 800 ° C. was used, the pellet shape did not become spherical, and the surface had protrusions like confetti. . FIG. 4 shows a drawing-substituting photograph in which an agglomerate granulated using a pulverized product of the heat-treated powder obtained at a heating temperature of 400 ° C.

これに対し、加熱温度を1100℃または1200℃として得られた熱処理粉末の粉砕物を用いた場合は、ペレットの形状は球状になった。加熱温度を1200℃として得られた熱処理粉末の粉砕物を用いて造粒したペレットを撮影した図面代用写真を図5に示す。   On the other hand, when the pulverized product of the heat-treated powder obtained at a heating temperature of 1100 ° C. or 1200 ° C. was used, the pellet shape was spherical. FIG. 5 shows a drawing-substituting photograph in which pellets granulated using a pulverized product of heat-treated powder obtained at a heating temperature of 1200 ° C. are photographed.

次に、加熱温度を1100℃または1200℃として得られた熱処理粉末を原料にして造粒して得られた湿潤ペレットについて、水分量(%)、塊成物1個あたりの圧潰強度(kg)、および空隙率(%)を測定した。結果を下記表2に示す。   Next, with respect to the wet pellets obtained by granulating the heat-treated powder obtained at a heating temperature of 1100 ° C. or 1200 ° C., the moisture content (%) and the crush strength per agglomerate (kg) , And porosity (%) was measured. The results are shown in Table 2 below.

圧潰強度は、2枚の平板間にペレットを1個設置し、ペレットが圧縮されるように平板に荷重を負荷してペレットの破壊時における荷重(圧潰荷重。単位はkg)を強度試験機で測定した。なお、圧潰荷重の測定は、10個のペレットについて行い、その平均値で示した。   For the crushing strength, one pellet is placed between two flat plates, and a load is applied to the flat plate so that the pellet is compressed. It was measured. In addition, the measurement of crushing load was performed about ten pellets, and was shown by the average value.

空隙率(%)は、ペレットを水銀中に浸漬してその浮力で測定した見掛比重値と、混合原料粉末の真比重値とから計算して求めた。   The porosity (%) was obtained by calculating from the apparent specific gravity value obtained by immersing the pellets in mercury and measuring the buoyancy and the true specific gravity value of the mixed raw material powder.

加熱温度を1100℃または1200℃として得られた熱処理粉末を原料として造粒した場合には、得られる湿潤ペレットに含まれる水分量、圧潰強度、空隙率は、ペレタイジングプラントで製造される生ペレットとほぼ同等になることが確認できた。   When the heat-treated powder obtained at a heating temperature of 1100 ° C. or 1200 ° C. is granulated as a raw material, the moisture content, crushing strength, and porosity contained in the obtained wet pellets are the same as those produced in the pelletizing plant. It was confirmed that it was almost the same as the pellet.

これらのペレットを加熱硬化処理後、例えば、還元性ガス雰囲気で加熱すれば、還元鉄を製造できる。また、上記熱処理粉末に炭素質還元剤やバインダー等を配合してペレットを調製し、これを加熱しても還元鉄を製造できる。   If these pellets are heated and cured in a reducing gas atmosphere, for example, reduced iron can be produced. Also, reduced iron can be produced by preparing pellets by mixing a carbonaceous reducing agent, a binder or the like with the heat-treated powder and heating the pellets.

以上の通り、本発明によれば、50%粒子径が2μm以下の酸化鉄含有粉末を、加熱温度900〜1200℃で熱処理することによって、造粒可能な粒度とすることができ、塊成物を製造できる。この塊成物は、鉄源として有効利用できる。   As described above, according to the present invention, an iron oxide-containing powder having a 50% particle size of 2 μm or less can be heat treated at a heating temperature of 900 to 1200 ° C. to obtain a granulated particle size. Can be manufactured. This agglomerate can be effectively used as an iron source.

Claims (9)

50%粒子径が2μm以下の酸化鉄含有粉末を、加熱温度900〜1200℃で熱処理する工程と、
得られた熱処理粉末を原料として造粒して塊成物を製造する工程と、
を含むことを特徴とする塊成物の製造方法。
A step of heat-treating an iron oxide-containing powder having a 50% particle size of 2 μm or less at a heating temperature of 900 to 1200 ° C .;
A process of granulating the obtained heat-treated powder as a raw material to produce an agglomerate;
The manufacturing method of the agglomerate characterized by including.
前記造粒は、転動造粒法によって行う請求項1に記載の製造方法。   The said granulation is a manufacturing method of Claim 1 performed by a rolling granulation method. 前記熱処理は、前記熱処理粉末の50%粒子径が4μm以上となるように行う請求項1または2に記載の製造方法。   The manufacturing method according to claim 1 or 2, wherein the heat treatment is performed such that a 50% particle diameter of the heat treated powder is 4 µm or more. 前記熱処理は、加熱時間を30分以上とする請求項1〜3のいずれかに記載の製造方法。   The said heat processing is a manufacturing method in any one of Claims 1-3 which makes heating time 30 minutes or more. 前記熱処理は、前記酸化鉄含有粉末を転動させつつ行う請求項1〜4のいずれかに記載の製造方法。   The manufacturing method according to claim 1, wherein the heat treatment is performed while rolling the iron oxide-containing powder. 前記酸化鉄含有粉末は、尾鉱である請求項1〜5のいずれかに記載の製造方法。   The method according to claim 1, wherein the iron oxide-containing powder is tailing. 前記尾鉱は、Ni含有鉱石からNiを回収した後の残渣である請求項6に記載の製造方法。   The manufacturing method according to claim 6, wherein the tailings are residues after recovering Ni from Ni-containing ore. 請求項1〜7のいずれかに記載の製造方法で得られた塊成物を加熱して還元鉄を製造することを特徴とする還元鉄の製造方法。   A reduced iron is produced by heating the agglomerate obtained by the production method according to claim 1 to produce reduced iron. 前記塊成物は、炭素質還元剤を更に含む請求項8に記載の製造方法。   The manufacturing method according to claim 8, wherein the agglomerate further contains a carbonaceous reducing agent.
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